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

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

data_3b
_database_code_depnum_ccdc_archive 'CCDC 1944621'
loop_
_audit_author_name
_audit_author_address
'Eleuterio Alvarez'
; Spanish National Research Council (CSIC) 
Spain
;
_audit_update_record             
;
2019-11-19 deposited with the CCDC.	2019-11-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C41 H49 N2 Ni P Si'
_chemical_formula_sum            'C41 H49 N2 Ni P Si'
_chemical_formula_weight         687.59

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'
Si Si 0.0817 0.0704 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   12.7840(5)
_cell_length_b                   18.6105(8)
_cell_length_c                   16.2525(6)
_cell_angle_alpha                90
_cell_angle_beta                 103.625(2)
_cell_angle_gamma                90
_cell_volume                     3757.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    9976
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      30.31

_exptl_crystal_description       priam
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_F_000             1464
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.621
_shelx_estimated_absorpt_T_min   0.836
_shelx_estimated_absorpt_T_max   0.886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6809
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   
; 
program SADABS, Bruker (2001). 
;
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
; 
 Bruker-Nonius X8kappa APEX II CCD area detector 
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_diffrn_detector_area_resol_mean 8.2
_diffrn_reflns_number            66822
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.133
_diffrn_reflns_theta_max         30.566
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             10664
_reflns_number_gt                8586
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0409P)²+1.1712P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10664
_refine_ls_number_parameters     422
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0327
_refine_ls_wR_factor_ref         0.0869
_refine_ls_wR_factor_gt          0.0796
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_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
Ni1 Ni 0.42709(2) 0.22073(2) 0.29620(2) 0.02490(5) Uani 1 1 d . . . . .
P1 P 0.51649(3) 0.31735(2) 0.30738(2) 0.02485(7) Uani 1 1 d . . . . .
Si1 Si 0.60624(3) 0.10141(2) 0.30668(3) 0.03943(10) Uani 1 1 d . . . . .
N1 N 0.33287(8) 0.27327(6) 0.35848(7) 0.0249(2) Uani 1 1 d . . . . .
N2 N 0.33756(9) 0.13452(6) 0.27312(8) 0.0328(3) Uani 1 1 d . . . . .
C1 C 0.36665(10) 0.33843(7) 0.39114(8) 0.0245(2) Uani 1 1 d . . . . .
C2 C 0.46023(11) 0.36794(7) 0.37695(8) 0.0278(3) Uani 1 1 d . . . . .
H2 H 0.490916 0.411377 0.402453 0.033 Uiso 1 1 calc R U . . .
C3 C 0.30791(11) 0.38333(7) 0.44256(8) 0.0279(3) Uani 1 1 d . . . . .
C4 C 0.19780(12) 0.39699(8) 0.41938(10) 0.0342(3) Uani 1 1 d . . . . .
H4 H 0.154639 0.374358 0.370681 0.041 Uiso 1 1 calc R U . . .
C5 C 0.15038(14) 0.44366(9) 0.46714(12) 0.0456(4) Uani 1 1 d . . . . .
H5 H 0.075289 0.452920 0.450170 0.055 Uiso 1 1 calc R U . . .
C6 C 0.21082(17) 0.47644(9) 0.53844(13) 0.0539(5) Uani 1 1 d . . . . .
H6 H 0.177973 0.508264 0.570534 0.065 Uiso 1 1 calc R U . . .
C7 C 0.31953(16) 0.46258(10) 0.56275(12) 0.0529(5) Uani 1 1 d . . . . .
H7 H 0.361693 0.484677 0.612239 0.064 Uiso 1 1 calc R U . . .
C8 C 0.36822(13) 0.41656(9) 0.51560(10) 0.0395(3) Uani 1 1 d . . . . .
H8 H 0.443336 0.407585 0.533212 0.047 Uiso 1 1 calc R U . . .
C9 C 0.23051(10) 0.24507(7) 0.36307(9) 0.0265(3) Uani 1 1 d . . . . .
C10 C 0.21154(11) 0.21790(7) 0.43920(10) 0.0316(3) Uani 1 1 d . . . . .
C11 C 0.11251(12) 0.18531(8) 0.43709(12) 0.0440(4) Uani 1 1 d . . . . .
H11 H 0.098576 0.167104 0.488072 0.053 Uiso 1 1 calc R U . . .
C12 C 0.03529(12) 0.17904(9) 0.36348(14) 0.0519(5) Uani 1 1 d . . . . .
H12 H -0.031195 0.156271 0.363563 0.062 Uiso 1 1 calc R U . . .
C13 C 0.05371(12) 0.20571(9) 0.28898(13) 0.0466(4) Uani 1 1 d . . . . .
H13 H -0.000578 0.201008 0.238107 0.056 Uiso 1 1 calc R U . . .
C14 C 0.15043(11) 0.23944(8) 0.28685(10) 0.0331(3) Uani 1 1 d . . . . .
C15 C 0.29260(13) 0.22185(9) 0.52386(10) 0.0396(3) Uani 1 1 d . . . . .
H15 H 0.358774 0.246266 0.515017 0.047 Uiso 1 1 calc R U . . .
C16 C 0.32488(18) 0.14710(11) 0.56164(13) 0.0586(5) Uani 1 1 d . . . . .
H16A H 0.260139 0.120371 0.565439 0.088 Uiso 1 1 calc R U . . .
H16B H 0.372069 0.152346 0.618332 0.088 Uiso 1 1 calc R U . . .
H16C H 0.363012 0.120945 0.525249 0.088 Uiso 1 1 calc R U . . .
C17 C 0.24852(17) 0.26613(10) 0.58813(12) 0.0528(4) Uani 1 1 d . . . . .
H17A H 0.227983 0.314048 0.564863 0.079 Uiso 1 1 calc R U . . .
H17B H 0.304146 0.270610 0.640877 0.079 Uiso 1 1 calc R U . . .
H17C H 0.185351 0.241947 0.599593 0.079 Uiso 1 1 calc R U . . .
C18 C 0.16916(14) 0.27008(8) 0.20446(10) 0.0410(4) Uani 1 1 d . . . . .
H18 H 0.244648 0.257767 0.202409 0.049 Uiso 1 1 calc R U . . .
C19 C 0.15974(18) 0.35189(10) 0.20112(11) 0.0555(5) Uani 1 1 d . . . . .
H19A H 0.087848 0.366086 0.206534 0.083 Uiso 1 1 calc R U . . .
H19B H 0.171203 0.369252 0.146997 0.083 Uiso 1 1 calc R U . . .
H19C H 0.214140 0.372828 0.247698 0.083 Uiso 1 1 calc R U . . .
C20 C 0.09494(18) 0.23868(12) 0.12488(13) 0.0646(6) Uani 1 1 d . . . . .
H20A H 0.020303 0.252022 0.123170 0.097 Uiso 1 1 calc R U . . .
H20B H 0.101598 0.186206 0.125834 0.097 Uiso 1 1 calc R U . . .
H20C H 0.115334 0.257667 0.074625 0.097 Uiso 1 1 calc R U . . .
C21 C 0.66225(10) 0.32244(7) 0.34512(9) 0.0278(3) Uani 1 1 d . . . . .
C22 C 0.70702(13) 0.31830(9) 0.43138(10) 0.0411(3) Uani 1 1 d . . . . .
H22 H 0.661516 0.315193 0.469789 0.049 Uiso 1 1 calc R U . . .
C23 C 0.81814(15) 0.31865(10) 0.46202(12) 0.0494(4) Uani 1 1 d . . . . .
H23 H 0.847982 0.315162 0.521214 0.059 Uiso 1 1 calc R U . . .
C24 C 0.88526(13) 0.32400(9) 0.40751(12) 0.0463(4) Uani 1 1 d . . . . .
H24 H 0.961138 0.324131 0.428772 0.056 Uiso 1 1 calc R U . . .
C25 C 0.84179(13) 0.32914(10) 0.32243(12) 0.0477(4) Uani 1 1 d . . . . .
H25 H 0.887853 0.333352 0.284560 0.057 Uiso 1 1 calc R U . . .
C26 C 0.73128(12) 0.32827(9) 0.29087(10) 0.0384(3) Uani 1 1 d . . . . .
H26 H 0.702322 0.331697 0.231546 0.046 Uiso 1 1 calc R U . . .
C27 C 0.49076(10) 0.36403(7) 0.20549(8) 0.0274(3) Uani 1 1 d . . . . .
C28 C 0.52101(13) 0.43512(8) 0.19980(10) 0.0382(3) Uani 1 1 d . . . . .
H28 H 0.563643 0.458462 0.248196 0.046 Uiso 1 1 calc R U . . .
C29 C 0.48967(15) 0.47232(9) 0.12429(11) 0.0458(4) Uani 1 1 d . . . . .
H29 H 0.510356 0.521101 0.121273 0.055 Uiso 1 1 calc R U . . .
C30 C 0.42850(14) 0.43887(10) 0.05336(11) 0.0439(4) Uani 1 1 d . . . . .
H30 H 0.405895 0.464865 0.001930 0.053 Uiso 1 1 calc R U . . .
C31 C 0.40044(14) 0.36825(10) 0.05718(10) 0.0440(4) Uani 1 1 d . . . . .
H31 H 0.359819 0.344813 0.008032 0.053 Uiso 1 1 calc R U . . .
C32 C 0.43136(12) 0.33086(8) 0.13290(10) 0.0371(3) Uani 1 1 d . . . . .
H32 H 0.411583 0.281821 0.135098 0.045 Uiso 1 1 calc R U . . .
C33 C 0.53254(11) 0.17594(7) 0.24222(10) 0.0325(3) Uani 1 1 d . . . . .
H33A H 0.495036 0.157185 0.185999 0.039 Uiso 1 1 calc R U . . .
H33B H 0.584752 0.212745 0.233433 0.039 Uiso 1 1 calc R U . . .
C34 C 0.74852(15) 0.10131(14) 0.29586(17) 0.0759(7) Uani 1 1 d . . . . .
H34A H 0.749486 0.095721 0.236089 0.114 Uiso 1 1 calc R U . . .
H34B H 0.787625 0.061348 0.328576 0.114 Uiso 1 1 calc R U . . .
H34C H 0.783079 0.146796 0.317252 0.114 Uiso 1 1 calc R U . . .
C35 C 0.54537(17) 0.01224(10) 0.26993(16) 0.0641(6) Uani 1 1 d . . . . .
H35A H 0.471106 0.010649 0.276410 0.096 Uiso 1 1 calc R U . . .
H35B H 0.587356 -0.026018 0.303906 0.096 Uiso 1 1 calc R U . . .
H35C H 0.545747 0.005371 0.210219 0.096 Uiso 1 1 calc R U . . .
C36 C 0.61110(19) 0.11089(14) 0.42237(13) 0.0693(6) Uani 1 1 d . . . . .
H36A H 0.646727 0.156154 0.443387 0.104 Uiso 1 1 calc R U . . .
H36B H 0.651434 0.070593 0.453410 0.104 Uiso 1 1 calc R U . . .
H36C H 0.537663 0.110888 0.430776 0.104 Uiso 1 1 calc R U . . .
C37 C 0.29401(13) 0.11296(9) 0.19354(12) 0.0438(4) Uani 1 1 d . . . . .
H37 H 0.310850 0.139047 0.148095 0.053 Uiso 1 1 calc R U . . .
C38 C 0.22570(15) 0.05444(10) 0.17475(16) 0.0605(6) Uani 1 1 d . . . . .
H38 H 0.195849 0.041010 0.117655 0.073 Uiso 1 1 calc R U . . .
C39 C 0.20208(16) 0.01641(10) 0.23992(18) 0.0685(7) Uani 1 1 d . . . . .
H39 H 0.155001 -0.023758 0.228799 0.082 Uiso 1 1 calc R U . . .
C40 C 0.24725(16) 0.03697(9) 0.32174(16) 0.0606(6) Uani 1 1 d . . . . .
H40 H 0.232704 0.010751 0.367946 0.073 Uiso 1 1 calc R U . . .
C41 C 0.31449(13) 0.09659(8) 0.33605(12) 0.0422(4) Uani 1 1 d . . . . .
H41 H 0.345109 0.110812 0.392753 0.051 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N2 1.9552(11) . ?
Ni1 C33 1.9593(13) . ?
Ni1 N1 2.0015(11) . ?
Ni1 P1 2.1153(4) . ?
P1 C2 1.7508(13) . ?
P1 C21 1.8218(14) . ?
P1 C27 1.8300(14) . ?
Si1 C33 1.8558(15) . ?
Si1 C34 1.8681(19) . ?
Si1 C35 1.8701(19) . ?
Si1 C36 1.875(2) . ?
N1 C1 1.3530(16) . ?
N1 C9 1.4280(15) . ?
N2 C41 1.332(2) . ?
N2 C37 1.343(2) . ?
C1 C2 1.3842(17) . ?
C1 C3 1.5021(17) . ?
C2 H2 0.9500 . ?
C3 C4 1.392(2) . ?
C3 C8 1.398(2) . ?
C4 C5 1.395(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.375(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.377(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.390(2) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.4096(19) . ?
C9 C14 1.413(2) . ?
C10 C11 1.3970(19) . ?
C10 C15 1.517(2) . ?
C11 C12 1.365(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.379(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.394(2) . ?
C13 H13 0.9500 . ?
C14 C18 1.525(2) . ?
C15 C16 1.537(2) . ?
C15 C17 1.538(2) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.527(2) . ?
C18 C20 1.528(2) . ?
C18 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.386(2) . ?
C21 C26 1.3909(19) . ?
C22 C23 1.390(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.374(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.367(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.385(2) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.3876(19) . ?
C27 C32 1.388(2) . ?
C28 C29 1.384(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.380(2) . ?
C29 H29 0.9500 . ?
C30 C31 1.368(2) . ?
C30 H30 0.9500 . ?
C31 C32 1.388(2) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.384(2) . ?
C37 H37 0.9500 . ?
C38 C39 1.365(3) . ?
C38 H38 0.9500 . ?
C39 C40 1.373(3) . ?
C39 H39 0.9500 . ?
C40 C41 1.389(2) . ?
C40 H40 0.9500 . ?
C41 H41 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ni1 C33 89.91(5) . . ?
N2 Ni1 N1 95.91(4) . . ?
C33 Ni1 N1 173.61(5) . . ?
N2 Ni1 P1 173.76(4) . . ?
C33 Ni1 P1 89.16(4) . . ?
N1 Ni1 P1 85.33(3) . . ?
C2 P1 C21 107.33(6) . . ?
C2 P1 C27 108.39(6) . . ?
C21 P1 C27 103.39(6) . . ?
C2 P1 Ni1 102.52(4) . . ?
C21 P1 Ni1 124.21(4) . . ?
C27 P1 Ni1 110.33(4) . . ?
C33 Si1 C34 108.89(9) . . ?
C33 Si1 C35 111.42(8) . . ?
C34 Si1 C35 108.07(11) . . ?
C33 Si1 C36 112.85(9) . . ?
C34 Si1 C36 106.95(11) . . ?
C35 Si1 C36 108.47(12) . . ?
C1 N1 C9 121.37(10) . . ?
C1 N1 Ni1 117.50(8) . . ?
C9 N1 Ni1 120.99(8) . . ?
C41 N2 C37 117.68(14) . . ?
C41 N2 Ni1 120.87(11) . . ?
C37 N2 Ni1 121.40(11) . . ?
N1 C1 C2 119.92(11) . . ?
N1 C1 C3 124.17(11) . . ?
C2 C1 C3 115.90(11) . . ?
C1 C2 P1 113.38(9) . . ?
C1 C2 H2 123.3 . . ?
P1 C2 H2 123.3 . . ?
C4 C3 C8 117.98(13) . . ?
C4 C3 C1 123.86(12) . . ?
C8 C3 C1 118.07(13) . . ?
C5 C4 C3 120.48(15) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C6 C5 C4 120.90(16) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C5 C6 C7 119.19(15) . . ?
C5 C6 H6 120.4 . . ?
C7 C6 H6 120.4 . . ?
C6 C7 C8 120.66(17) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
C7 C8 C3 120.76(16) . . ?
C7 C8 H8 119.6 . . ?
C3 C8 H8 119.6 . . ?
C10 C9 C14 120.27(12) . . ?
C10 C9 N1 121.80(12) . . ?
C14 C9 N1 117.72(12) . . ?
C11 C10 C9 118.46(14) . . ?
C11 C10 C15 117.70(14) . . ?
C9 C10 C15 123.84(12) . . ?
C12 C11 C10 121.52(16) . . ?
C12 C11 H11 119.2 . . ?
C10 C11 H11 119.2 . . ?
C11 C12 C13 120.06(14) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C12 C13 C14 121.30(16) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C13 C14 C9 118.38(15) . . ?
C13 C14 C18 120.90(15) . . ?
C9 C14 C18 120.72(13) . . ?
C10 C15 C16 112.34(14) . . ?
C10 C15 C17 111.15(14) . . ?
C16 C15 C17 108.69(14) . . ?
C10 C15 H15 108.2 . . ?
C16 C15 H15 108.2 . . ?
C17 C15 H15 108.2 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 C19 112.11(13) . . ?
C14 C18 C20 113.91(16) . . ?
C19 C18 C20 108.85(15) . . ?
C14 C18 H18 107.2 . . ?
C19 C18 H18 107.2 . . ?
C20 C18 H18 107.2 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C26 118.24(13) . . ?
C22 C21 P1 118.92(11) . . ?
C26 C21 P1 122.82(11) . . ?
C21 C22 C23 120.37(15) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 H22 119.8 . . ?
C24 C23 C22 120.66(17) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C25 C24 C23 119.37(15) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
C24 C25 C26 120.67(16) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C25 C26 C21 120.68(15) . . ?
C25 C26 H26 119.7 . . ?
C21 C26 H26 119.7 . . ?
C28 C27 C32 118.20(13) . . ?
C28 C27 P1 121.30(11) . . ?
C32 C27 P1 120.24(10) . . ?
C29 C28 C27 120.61(15) . . ?
C29 C28 H28 119.7 . . ?
C27 C28 H28 119.7 . . ?
C30 C29 C28 120.27(15) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C31 C30 C29 119.93(15) . . ?
C31 C30 H30 120.0 . . ?
C29 C30 H30 120.0 . . ?
C30 C31 C32 119.94(16) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C31 C32 C27 121.01(14) . . ?
C31 C32 H32 119.5 . . ?
C27 C32 H32 119.5 . . ?
Si1 C33 Ni1 112.12(7) . . ?
Si1 C33 H33A 109.2 . . ?
Ni1 C33 H33A 109.2 . . ?
Si1 C33 H33B 109.2 . . ?
Ni1 C33 H33B 109.2 . . ?
H33A C33 H33B 107.9 . . ?
Si1 C34 H34A 109.5 . . ?
Si1 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
Si1 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
Si1 C35 H35A 109.5 . . ?
Si1 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
Si1 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
Si1 C36 H36A 109.5 . . ?
Si1 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
Si1 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N2 C37 C38 122.97(19) . . ?
N2 C37 H37 118.5 . . ?
C38 C37 H37 118.5 . . ?
C39 C38 C37 118.7(2) . . ?
C39 C38 H38 120.7 . . ?
C37 C38 H38 120.7 . . ?
C38 C39 C40 119.15(17) . . ?
C38 C39 H39 120.4 . . ?
C40 C39 H39 120.4 . . ?
C39 C40 C41 119.1(2) . . ?
C39 C40 H40 120.4 . . ?
C41 C40 H40 120.4 . . ?
N2 C41 C40 122.34(18) . . ?
N2 C41 H41 118.8 . . ?
C40 C41 H41 118.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 N1 C1 C2 -172.34(12) . . . . ?
Ni1 N1 C1 C2 3.44(16) . . . . ?
C9 N1 C1 C3 6.87(19) . . . . ?
Ni1 N1 C1 C3 -177.35(10) . . . . ?
N1 C1 C2 P1 5.76(17) . . . . ?
C3 C1 C2 P1 -173.51(9) . . . . ?
C21 P1 C2 C1 -143.24(10) . . . . ?
C27 P1 C2 C1 105.70(11) . . . . ?
Ni1 P1 C2 C1 -10.97(11) . . . . ?
N1 C1 C3 C4 -47.47(19) . . . . ?
C2 C1 C3 C4 131.77(14) . . . . ?
N1 C1 C3 C8 136.14(14) . . . . ?
C2 C1 C3 C8 -44.62(18) . . . . ?
C8 C3 C4 C5 1.3(2) . . . . ?
C1 C3 C4 C5 -175.12(13) . . . . ?
C3 C4 C5 C6 -0.8(2) . . . . ?
C4 C5 C6 C7 -0.2(3) . . . . ?
C5 C6 C7 C8 0.6(3) . . . . ?
C6 C7 C8 C3 0.0(3) . . . . ?
C4 C3 C8 C7 -0.9(2) . . . . ?
C1 C3 C8 C7 175.72(15) . . . . ?
C1 N1 C9 C10 -74.65(17) . . . . ?
Ni1 N1 C9 C10 109.72(12) . . . . ?
C1 N1 C9 C14 110.66(14) . . . . ?
Ni1 N1 C9 C14 -64.97(14) . . . . ?
C14 C9 C10 C11 0.3(2) . . . . ?
N1 C9 C10 C11 -174.30(12) . . . . ?
C14 C9 C10 C15 -179.76(13) . . . . ?
N1 C9 C10 C15 5.7(2) . . . . ?
C9 C10 C11 C12 0.5(2) . . . . ?
C15 C10 C11 C12 -179.53(15) . . . . ?
C10 C11 C12 C13 -0.6(3) . . . . ?
C11 C12 C13 C14 -0.1(3) . . . . ?
C12 C13 C14 C9 0.7(2) . . . . ?
C12 C13 C14 C18 -178.78(14) . . . . ?
C10 C9 C14 C13 -0.84(19) . . . . ?
N1 C9 C14 C13 173.94(12) . . . . ?
C10 C9 C14 C18 178.69(12) . . . . ?
N1 C9 C14 C18 -6.54(18) . . . . ?
C11 C10 C15 C16 60.49(19) . . . . ?
C9 C10 C15 C16 -119.48(16) . . . . ?
C11 C10 C15 C17 -61.54(18) . . . . ?
C9 C10 C15 C17 118.48(15) . . . . ?
C13 C14 C18 C19 104.08(18) . . . . ?
C9 C14 C18 C19 -75.43(19) . . . . ?
C13 C14 C18 C20 -20.1(2) . . . . ?
C9 C14 C18 C20 160.40(14) . . . . ?
C2 P1 C21 C22 40.78(13) . . . . ?
C27 P1 C21 C22 155.23(12) . . . . ?
Ni1 P1 C21 C22 -78.35(12) . . . . ?
C2 P1 C21 C26 -141.12(12) . . . . ?
C27 P1 C21 C26 -26.66(14) . . . . ?
Ni1 P1 C21 C26 99.76(12) . . . . ?
C26 C21 C22 C23 -1.2(2) . . . . ?
P1 C21 C22 C23 177.01(13) . . . . ?
C21 C22 C23 C24 0.8(3) . . . . ?
C22 C23 C24 C25 0.1(3) . . . . ?
C23 C24 C25 C26 -0.6(3) . . . . ?
C24 C25 C26 C21 0.3(3) . . . . ?
C22 C21 C26 C25 0.7(2) . . . . ?
P1 C21 C26 C25 -177.45(13) . . . . ?
C2 P1 C27 C28 54.55(13) . . . . ?
C21 P1 C27 C28 -59.13(13) . . . . ?
Ni1 P1 C27 C28 166.08(11) . . . . ?
C2 P1 C27 C32 -119.47(12) . . . . ?
C21 P1 C27 C32 126.84(12) . . . . ?
Ni1 P1 C27 C32 -7.95(13) . . . . ?
C32 C27 C28 C29 2.0(2) . . . . ?
P1 C27 C28 C29 -172.13(13) . . . . ?
C27 C28 C29 C30 -0.5(3) . . . . ?
C28 C29 C30 C31 -1.3(3) . . . . ?
C29 C30 C31 C32 1.5(3) . . . . ?
C30 C31 C32 C27 0.0(3) . . . . ?
C28 C27 C32 C31 -1.7(2) . . . . ?
P1 C27 C32 C31 172.46(12) . . . . ?
C34 Si1 C33 Ni1 -143.93(11) . . . . ?
C35 Si1 C33 Ni1 96.97(11) . . . . ?
C36 Si1 C33 Ni1 -25.34(12) . . . . ?
C41 N2 C37 C38 1.1(2) . . . . ?
Ni1 N2 C37 C38 -176.50(12) . . . . ?
N2 C37 C38 C39 -0.6(3) . . . . ?
C37 C38 C39 C40 -0.5(3) . . . . ?
C38 C39 C40 C41 1.0(3) . . . . ?
C37 N2 C41 C40 -0.6(2) . . . . ?
Ni1 N2 C41 C40 177.06(12) . . . . ?
C39 C40 C41 N2 -0.5(3) . . . . ?

_refine_diff_density_max         0.321
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.047

####################################################################### 
# 
# 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_7b
_database_code_depnum_ccdc_archive 'CCDC 1944624'
loop_
_audit_author_name
_audit_author_address
'Eleuterio Alvarez'
; Spanish National Research Council (CSIC) 
Spain
;
_audit_update_record             
;
2019-11-19 deposited with the CCDC.	2019-11-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H41 Br N Ni O P'
_chemical_formula_sum            'C40 H41 Br N Ni O P'
_chemical_formula_weight         721.33

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'

_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                   9.9701(2)
_cell_length_b                   14.6823(3)
_cell_length_c                   12.4003(3)
_cell_angle_alpha                90
_cell_angle_beta                 108.9940(10)
_cell_angle_gamma                90
_cell_volume                     1716.37(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    9932
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      30.49

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_F_000             748
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    1.808
_shelx_estimated_absorpt_T_min   0.661
_shelx_estimated_absorpt_T_max   0.737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6436
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   
; 
program SADABS, Bruker (2001). 
;
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
 Bruker-Nonius X8kappa APEX II CCD area detector
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_diffrn_detector_area_resol_mean 8.2
_diffrn_reflns_number            24230
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.160
_diffrn_reflns_theta_max         30.511
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.788
_diffrn_reflns_point_group_measured_fraction_full 0.839
_reflns_number_total             8272
_reflns_number_gt                7647
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.529
_reflns_Friedel_fraction_max     0.566
_reflns_Friedel_fraction_full    0.666

_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. Completness statistics refer to single and 
 composite reflections containing twin component 1 only. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
 Refined as a 2-component inversion twin. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0236P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   -0.004(6)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8272
_refine_ls_number_parameters     412
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0236
_refine_ls_wR_factor_ref         0.0560
_refine_ls_wR_factor_gt          0.0549
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.34618(2) 0.44447(2) 0.64872(2) 0.01885(6) Uani 1 1 d . . . . .
Br1 Br 0.29217(2) 0.35557(2) 0.78410(2) 0.03464(6) Uani 1 1 d . . . . .
P1 P 0.35694(5) 0.53858(3) 0.52365(4) 0.01885(10) Uani 1 1 d . . . . .
O1 O -0.18595(19) 0.19974(16) 0.26936(18) 0.0514(5) Uani 1 1 d . . . . .
N1 N 0.49531(17) 0.52351(11) 0.75893(14) 0.0197(3) Uani 1 1 d . . . . .
C1 C 0.5718(2) 0.49001(13) 0.87303(17) 0.0216(4) Uani 1 1 d . . . . .
C2 C 0.5309(2) 0.51858(15) 0.96485(18) 0.0257(4) Uani 1 1 d . . . . .
C3 C 0.5993(3) 0.47937(17) 1.07141(19) 0.0341(5) Uani 1 1 d . . . . .
H3 H 0.573185 0.497736 1.135290 0.041 Uiso 1 1 calc R U . . .
C4 C 0.7045(3) 0.41423(17) 1.0858(2) 0.0368(6) Uani 1 1 d . . . . .
H4 H 0.749283 0.388082 1.158798 0.044 Uiso 1 1 calc R U . . .
C5 C 0.7438(2) 0.38765(16) 0.9939(2) 0.0317(5) Uani 1 1 d . . . . .
H5 H 0.816493 0.343446 1.004460 0.038 Uiso 1 1 calc R U . . .
C6 C 0.6791(2) 0.42419(14) 0.88564(19) 0.0255(4) Uani 1 1 d . . . . .
C7 C 0.4196(3) 0.59163(17) 0.9564(2) 0.0331(5) Uani 1 1 d . . . . .
H7 H 0.379560 0.610559 0.874695 0.040 Uiso 1 1 calc R U . . .
C8 C 0.4879(4) 0.67608(19) 1.0268(2) 0.0489(7) Uani 1 1 d . . . . .
H8A H 0.515503 0.661611 1.108282 0.073 Uiso 1 1 calc R U . . .
H8B H 0.419604 0.726378 1.009300 0.073 Uiso 1 1 calc R U . . .
H8C H 0.572163 0.693949 1.007636 0.073 Uiso 1 1 calc R U . . .
C9 C 0.2970(3) 0.5566(2) 0.9942(3) 0.0476(7) Uani 1 1 d . . . . .
H9A H 0.258899 0.500486 0.952686 0.071 Uiso 1 1 calc R U . . .
H9B H 0.222096 0.602802 0.977648 0.071 Uiso 1 1 calc R U . . .
H9C H 0.331664 0.544127 1.076252 0.071 Uiso 1 1 calc R U . . .
C10 C 0.7259(2) 0.39295(15) 0.7871(2) 0.0300(5) Uani 1 1 d . . . . .
H10 H 0.689205 0.437918 0.723747 0.036 Uiso 1 1 calc R U . . .
C11 C 0.8882(3) 0.3887(2) 0.8170(3) 0.0461(7) Uani 1 1 d . . . . .
H11A H 0.930662 0.443662 0.859252 0.069 Uiso 1 1 calc R U . . .
H11B H 0.912512 0.384910 0.746679 0.069 Uiso 1 1 calc R U . . .
H11C H 0.924637 0.334870 0.864133 0.069 Uiso 1 1 calc R U . . .
C12 C 0.6627(3) 0.30031(18) 0.7429(2) 0.0397(6) Uani 1 1 d . . . . .
H12A H 0.699216 0.254386 0.802599 0.059 Uiso 1 1 calc R U . . .
H12B H 0.688977 0.283708 0.675865 0.059 Uiso 1 1 calc R U . . .
H12C H 0.559101 0.303276 0.721688 0.059 Uiso 1 1 calc R U . . .
C13 C 0.5158(2) 0.60527(13) 0.72988(17) 0.0207(4) Uani 1 1 d . . . . .
C14 C 0.4211(2) 0.63855(13) 0.61448(17) 0.0219(4) Uani 1 1 d . . . . .
H14A H 0.475179 0.679034 0.579778 0.026 Uiso 1 1 calc R U . . .
H14B H 0.340046 0.673266 0.623027 0.026 Uiso 1 1 calc R U . . .
C15 C 0.6193(2) 0.67278(14) 0.79752(18) 0.0257(4) Uani 1 1 d . . . . .
C16 C 0.5777(3) 0.76401(17) 0.7919(2) 0.0404(6) Uani 1 1 d . . . . .
H16 H 0.484236 0.780587 0.746694 0.048 Uiso 1 1 calc R U . . .
C17 C 0.6705(3) 0.83030(18) 0.8511(3) 0.0583(10) Uani 1 1 d . . . . .
H17 H 0.640357 0.891918 0.847732 0.070 Uiso 1 1 calc R U . . .
C18 C 0.8080(4) 0.8069(2) 0.9157(3) 0.0599(10) Uani 1 1 d . . . . .
H18 H 0.872190 0.852527 0.956351 0.072 Uiso 1 1 calc R U . . .
C19 C 0.8514(3) 0.7178(2) 0.9210(3) 0.0478(7) Uani 1 1 d . . . . .
H19 H 0.946081 0.702256 0.964430 0.057 Uiso 1 1 calc R U . . .
C20 C 0.7578(3) 0.65033(16) 0.8634(2) 0.0323(5) Uani 1 1 d . . . . .
H20 H 0.788222 0.588676 0.868856 0.039 Uiso 1 1 calc R U . . .
C21 C 0.4933(2) 0.52088(14) 0.45837(17) 0.0218(4) Uani 1 1 d . . . . .
C22 C 0.5773(2) 0.44373(18) 0.4862(2) 0.0328(5) Uani 1 1 d . . . . .
H22 H 0.555329 0.396953 0.530679 0.039 Uiso 1 1 calc R U . . .
C23 C 0.6942(3) 0.4349(2) 0.4489(2) 0.0425(6) Uani 1 1 d . . . . .
H23 H 0.751995 0.382004 0.468531 0.051 Uiso 1 1 calc R U . . .
C24 C 0.7267(3) 0.5020(2) 0.3840(2) 0.0365(5) Uani 1 1 d . . . . .
H24 H 0.806897 0.495469 0.359206 0.044 Uiso 1 1 calc R U . . .
C25 C 0.6423(2) 0.57905(18) 0.3547(2) 0.0332(5) Uani 1 1 d . . . . .
H25 H 0.664577 0.625647 0.310117 0.040 Uiso 1 1 calc R U . . .
C26 C 0.5250(2) 0.58768(16) 0.3909(2) 0.0290(5) Uani 1 1 d . . . . .
H26 H 0.465681 0.639758 0.369370 0.035 Uiso 1 1 calc R U . . .
C27 C 0.2033(2) 0.57691(15) 0.40752(17) 0.0236(4) Uani 1 1 d . . . . .
C28 C 0.1642(3) 0.5304(2) 0.3043(2) 0.0398(6) Uani 1 1 d . . . . .
H28 H 0.220768 0.481378 0.293785 0.048 Uiso 1 1 calc R U . . .
C29 C 0.0426(3) 0.5555(3) 0.2165(2) 0.0530(8) Uani 1 1 d . . . . .
H29 H 0.016176 0.523547 0.146088 0.064 Uiso 1 1 calc R U . . .
C30 C -0.0401(3) 0.6271(2) 0.2316(2) 0.0477(7) Uani 1 1 d . . . . .
H30 H -0.123046 0.644074 0.171271 0.057 Uiso 1 1 calc R U . . .
C31 C -0.0031(3) 0.6733(2) 0.3326(2) 0.0406(6) Uani 1 1 d . . . . .
H31 H -0.060135 0.722377 0.342407 0.049 Uiso 1 1 calc R U . . .
C32 C 0.1185(3) 0.64846(17) 0.4213(2) 0.0313(5) Uani 1 1 d . . . . .
H32 H 0.143657 0.680528 0.491628 0.038 Uiso 1 1 calc R U . . .
C33 C 0.2249(2) 0.37116(13) 0.53281(17) 0.0223(4) Uani 1 1 d . . . . .
C34 C 0.0790(2) 0.38809(15) 0.4840(2) 0.0291(5) Uani 1 1 d . . . . .
H34 H 0.039937 0.442192 0.503459 0.035 Uiso 1 1 calc R U . . .
C35 C -0.0083(2) 0.32760(16) 0.40840(19) 0.0285(5) Uani 1 1 d . . . . .
H35 H -0.106199 0.341564 0.375599 0.034 Uiso 1 1 calc R U . . .
C36 C 0.0431(2) 0.24651(15) 0.37870(18) 0.0254(4) Uani 1 1 d . . . . .
C37 C 0.1889(2) 0.22986(16) 0.4240(2) 0.0321(5) Uani 1 1 d . . . . .
H37 H 0.227565 0.175706 0.404261 0.038 Uiso 1 1 calc R U . . .
C38 C 0.2773(2) 0.29240(16) 0.4979(2) 0.0317(5) Uani 1 1 d . . . . .
H38 H 0.376466 0.281119 0.525391 0.038 Uiso 1 1 calc R U . . .
C39 C -0.0598(3) 0.17969(18) 0.3090(2) 0.0325(5) Uani 1 1 d . . . . .
C40 C -0.0113(3) 0.0861(2) 0.2934(3) 0.0494(7) Uani 1 1 d . . . . .
H40A H -0.093897 0.046631 0.260873 0.074 Uiso 1 1 calc R U . . .
H40B H 0.047131 0.061759 0.367344 0.074 Uiso 1 1 calc R U . . .
H40C H 0.044873 0.088308 0.241596 0.074 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C33 1.8855(19) . ?
Ni1 N1 2.0255(16) . ?
Ni1 P1 2.1058(6) . ?
Ni1 Br1 2.3239(3) . ?
P1 C21 1.814(2) . ?
P1 C27 1.817(2) . ?
P1 C14 1.834(2) . ?
O1 C39 1.228(3) . ?
N1 C13 1.289(3) . ?
N1 C1 1.457(2) . ?
C1 C2 1.393(3) . ?
C1 C6 1.411(3) . ?
C2 C3 1.398(3) . ?
C2 C7 1.522(3) . ?
C3 C4 1.387(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.377(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.394(3) . ?
C5 H5 0.9500 . ?
C6 C10 1.515(3) . ?
C7 C9 1.533(4) . ?
C7 C8 1.542(4) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C12 1.524(3) . ?
C10 C11 1.538(4) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C15 1.479(3) . ?
C13 C14 1.516(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C20 1.396(3) . ?
C15 C16 1.397(3) . ?
C16 C17 1.378(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.387(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.372(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.389(3) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C22 1.384(3) . ?
C21 C26 1.390(3) . ?
C22 C23 1.392(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.377(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.386(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.389(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.389(3) . ?
C27 C32 1.393(3) . ?
C28 C29 1.390(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.385(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.366(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.394(3) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C38 1.394(3) . ?
C33 C34 1.404(3) . ?
C34 C35 1.376(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.392(3) . ?
C35 H35 0.9500 . ?
C36 C37 1.399(3) . ?
C36 C39 1.478(3) . ?
C37 C38 1.391(3) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C40 1.491(4) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?

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
C33 Ni1 N1 171.57(8) . . ?
C33 Ni1 P1 89.25(6) . . ?
N1 Ni1 P1 85.34(5) . . ?
C33 Ni1 Br1 89.32(6) . . ?
N1 Ni1 Br1 97.25(5) . . ?
P1 Ni1 Br1 168.499(19) . . ?
C21 P1 C27 104.60(10) . . ?
C21 P1 C14 103.09(10) . . ?
C27 P1 C14 105.93(9) . . ?
C21 P1 Ni1 117.39(7) . . ?
C27 P1 Ni1 123.71(7) . . ?
C14 P1 Ni1 99.44(7) . . ?
C13 N1 C1 120.37(16) . . ?
C13 N1 Ni1 119.56(13) . . ?
C1 N1 Ni1 119.94(12) . . ?
C2 C1 C6 121.88(19) . . ?
C2 C1 N1 119.47(18) . . ?
C6 C1 N1 118.49(19) . . ?
C1 C2 C3 117.8(2) . . ?
C1 C2 C7 123.83(19) . . ?
C3 C2 C7 118.4(2) . . ?
C4 C3 C2 121.4(2) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C5 C4 C3 119.7(2) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 121.4(2) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C5 C6 C1 117.8(2) . . ?
C5 C6 C10 119.5(2) . . ?
C1 C6 C10 122.65(19) . . ?
C2 C7 C9 112.2(2) . . ?
C2 C7 C8 110.5(2) . . ?
C9 C7 C8 110.2(2) . . ?
C2 C7 H7 107.9 . . ?
C9 C7 H7 107.9 . . ?
C8 C7 H7 107.9 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C10 C12 111.1(2) . . ?
C6 C10 C11 113.2(2) . . ?
C12 C10 C11 109.3(2) . . ?
C6 C10 H10 107.7 . . ?
C12 C10 H10 107.7 . . ?
C11 C10 H10 107.7 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N1 C13 C15 127.62(18) . . ?
N1 C13 C14 117.23(17) . . ?
C15 C13 C14 115.12(17) . . ?
C13 C14 P1 107.90(13) . . ?
C13 C14 H14A 110.1 . . ?
P1 C14 H14A 110.1 . . ?
C13 C14 H14B 110.1 . . ?
P1 C14 H14B 110.1 . . ?
H14A C14 H14B 108.4 . . ?
C20 C15 C16 118.4(2) . . ?
C20 C15 C13 123.27(19) . . ?
C16 C15 C13 118.25(19) . . ?
C17 C16 C15 120.9(2) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C16 C17 C18 119.9(3) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C19 C18 C17 120.1(2) . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C18 C19 C20 120.5(3) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
C19 C20 C15 120.2(2) . . ?
C19 C20 H20 119.9 . . ?
C15 C20 H20 119.9 . . ?
C22 C21 C26 119.4(2) . . ?
C22 C21 P1 119.12(16) . . ?
C26 C21 P1 121.15(17) . . ?
C21 C22 C23 119.8(2) . . ?
C21 C22 H22 120.1 . . ?
C23 C22 H22 120.1 . . ?
C24 C23 C22 120.6(2) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C23 C24 C25 119.9(2) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C25 C26 119.5(2) . . ?
C24 C25 H25 120.2 . . ?
C26 C25 H25 120.2 . . ?
C25 C26 C21 120.7(2) . . ?
C25 C26 H26 119.7 . . ?
C21 C26 H26 119.7 . . ?
C28 C27 C32 118.9(2) . . ?
C28 C27 P1 119.29(18) . . ?
C32 C27 P1 121.67(17) . . ?
C27 C28 C29 120.2(3) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
C30 C29 C28 120.1(3) . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C31 C30 C29 120.4(2) . . ?
C31 C30 H30 119.8 . . ?
C29 C30 H30 119.8 . . ?
C30 C31 C32 120.0(3) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C27 C32 C31 120.4(2) . . ?
C27 C32 H32 119.8 . . ?
C31 C32 H32 119.8 . . ?
C38 C33 C34 116.93(18) . . ?
C38 C33 Ni1 119.90(15) . . ?
C34 C33 Ni1 123.01(16) . . ?
C35 C34 C33 121.1(2) . . ?
C35 C34 H34 119.5 . . ?
C33 C34 H34 119.5 . . ?
C34 C35 C36 121.8(2) . . ?
C34 C35 H35 119.1 . . ?
C36 C35 H35 119.1 . . ?
C35 C36 C37 117.81(19) . . ?
C35 C36 C39 118.5(2) . . ?
C37 C36 C39 123.5(2) . . ?
C38 C37 C36 120.1(2) . . ?
C38 C37 H37 119.9 . . ?
C36 C37 H37 119.9 . . ?
C37 C38 C33 122.1(2) . . ?
C37 C38 H38 119.0 . . ?
C33 C38 H38 119.0 . . ?
O1 C39 C36 120.0(2) . . ?
O1 C39 C40 120.2(2) . . ?
C36 C39 C40 119.7(2) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?

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
C13 N1 C1 C2 75.7(3) . . . . ?
Ni1 N1 C1 C2 -100.12(19) . . . . ?
C13 N1 C1 C6 -108.8(2) . . . . ?
Ni1 N1 C1 C6 75.4(2) . . . . ?
C6 C1 C2 C3 -0.4(3) . . . . ?
N1 C1 C2 C3 174.95(19) . . . . ?
C6 C1 C2 C7 177.8(2) . . . . ?
N1 C1 C2 C7 -6.9(3) . . . . ?
C1 C2 C3 C4 0.0(4) . . . . ?
C7 C2 C3 C4 -178.2(2) . . . . ?
C2 C3 C4 C5 0.4(4) . . . . ?
C3 C4 C5 C6 -0.6(4) . . . . ?
C4 C5 C6 C1 0.3(3) . . . . ?
C4 C5 C6 C10 179.9(2) . . . . ?
C2 C1 C6 C5 0.2(3) . . . . ?
N1 C1 C6 C5 -175.15(18) . . . . ?
C2 C1 C6 C10 -179.40(19) . . . . ?
N1 C1 C6 C10 5.2(3) . . . . ?
C1 C2 C7 C9 122.4(2) . . . . ?
C3 C2 C7 C9 -59.4(3) . . . . ?
C1 C2 C7 C8 -114.1(2) . . . . ?
C3 C2 C7 C8 64.1(3) . . . . ?
C5 C6 C10 C12 78.1(3) . . . . ?
C1 C6 C10 C12 -102.3(2) . . . . ?
C5 C6 C10 C11 -45.3(3) . . . . ?
C1 C6 C10 C11 134.3(2) . . . . ?
C1 N1 C13 C15 4.6(3) . . . . ?
Ni1 N1 C13 C15 -179.61(17) . . . . ?
C1 N1 C13 C14 -173.61(18) . . . . ?
Ni1 N1 C13 C14 2.2(3) . . . . ?
N1 C13 C14 P1 -24.5(2) . . . . ?
C15 C13 C14 P1 157.10(16) . . . . ?
C21 P1 C14 C13 -88.68(16) . . . . ?
C27 P1 C14 C13 161.72(15) . . . . ?
Ni1 P1 C14 C13 32.48(15) . . . . ?
N1 C13 C15 C20 40.7(4) . . . . ?
C14 C13 C15 C20 -141.1(2) . . . . ?
N1 C13 C15 C16 -141.6(3) . . . . ?
C14 C13 C15 C16 36.6(3) . . . . ?
C20 C15 C16 C17 -0.8(5) . . . . ?
C13 C15 C16 C17 -178.6(3) . . . . ?
C15 C16 C17 C18 1.2(5) . . . . ?
C16 C17 C18 C19 -0.3(6) . . . . ?
C17 C18 C19 C20 -1.0(6) . . . . ?
C18 C19 C20 C15 1.3(5) . . . . ?
C16 C15 C20 C19 -0.4(4) . . . . ?
C13 C15 C20 C19 177.3(3) . . . . ?
C27 P1 C21 C22 -136.61(18) . . . . ?
C14 P1 C21 C22 112.80(18) . . . . ?
Ni1 P1 C21 C22 4.7(2) . . . . ?
C27 P1 C21 C26 50.4(2) . . . . ?
C14 P1 C21 C26 -60.20(19) . . . . ?
Ni1 P1 C21 C26 -168.27(15) . . . . ?
C26 C21 C22 C23 1.6(3) . . . . ?
P1 C21 C22 C23 -171.5(2) . . . . ?
C21 C22 C23 C24 -0.4(4) . . . . ?
C22 C23 C24 C25 -0.3(4) . . . . ?
C23 C24 C25 C26 -0.3(4) . . . . ?
C24 C25 C26 C21 1.5(4) . . . . ?
C22 C21 C26 C25 -2.2(3) . . . . ?
P1 C21 C26 C25 170.81(18) . . . . ?
C21 P1 C27 C28 46.7(2) . . . . ?
C14 P1 C27 C28 155.3(2) . . . . ?
Ni1 P1 C27 C28 -91.5(2) . . . . ?
C21 P1 C27 C32 -137.12(19) . . . . ?
C14 P1 C27 C32 -28.6(2) . . . . ?
Ni1 P1 C27 C32 84.7(2) . . . . ?
C32 C27 C28 C29 0.2(4) . . . . ?
P1 C27 C28 C29 176.5(2) . . . . ?
C27 C28 C29 C30 0.0(5) . . . . ?
C28 C29 C30 C31 -0.1(5) . . . . ?
C29 C30 C31 C32 -0.1(5) . . . . ?
C28 C27 C32 C31 -0.4(4) . . . . ?
P1 C27 C32 C31 -176.6(2) . . . . ?
C30 C31 C32 C27 0.4(4) . . . . ?
P1 Ni1 C33 C38 103.88(19) . . . . ?
Br1 Ni1 C33 C38 -87.54(19) . . . . ?
P1 Ni1 C33 C34 -80.90(18) . . . . ?
Br1 Ni1 C33 C34 87.69(18) . . . . ?
C38 C33 C34 C35 2.3(3) . . . . ?
Ni1 C33 C34 C35 -173.03(19) . . . . ?
C33 C34 C35 C36 1.3(4) . . . . ?
C34 C35 C36 C37 -3.1(4) . . . . ?
C34 C35 C36 C39 172.1(2) . . . . ?
C35 C36 C37 C38 1.2(4) . . . . ?
C39 C36 C37 C38 -173.7(2) . . . . ?
C36 C37 C38 C33 2.5(4) . . . . ?
C34 C33 C38 C37 -4.2(4) . . . . ?
Ni1 C33 C38 C37 171.3(2) . . . . ?
C35 C36 C39 O1 7.0(4) . . . . ?
C37 C36 C39 O1 -178.1(3) . . . . ?
C35 C36 C39 C40 -169.1(3) . . . . ?
C37 C36 C39 C40 5.8(4) . . . . ?

_refine_diff_density_max         0.386
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.050

####################################################################### 
# 
# 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_16
_database_code_depnum_ccdc_archive 'CCDC 1944625'
loop_
_audit_author_name
_audit_author_address
'Eleuterio Alvarez'
; Spanish National Research Council (CSIC) 
Spain
;
_audit_update_record             
;
2019-11-19 deposited with the CCDC.	2019-11-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H126 N2 Na2 Ni2 O8 P2'
_chemical_formula_sum            'C84 H126 N2 Na2 Ni2 O8 P2'
_chemical_formula_weight         1517.20

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'
Na Na 0.0362 0.0249 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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'
'-x, -y, -z'

_cell_length_a                   11.604(6)
_cell_length_b                   12.092(7)
_cell_length_c                   18.006(10)
_cell_angle_alpha                82.74(3)
_cell_angle_beta                 75.53(2)
_cell_angle_gamma                64.70(3)
_cell_volume                     2211(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    253(2)
_cell_measurement_reflns_used    5862
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      26.35

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_F_000             816
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.522
_shelx_estimated_absorpt_T_min   0.903
_shelx_estimated_absorpt_T_max   0.950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7002
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   
;
program SADABS, Bruker (2001).
;
_diffrn_ambient_temperature      253(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
 Bruker-Nonius X8kappa APEX II CCD area detector
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_diffrn_detector_area_resol_mean 8.2
_diffrn_reflns_number            31181
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.863
_diffrn_reflns_theta_max         30.492
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             13268
_reflns_number_gt                7487
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0805P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13268
_refine_ls_number_parameters     559
_refine_ls_number_restraints     485
_refine_ls_R_factor_all          0.1043
_refine_ls_R_factor_gt           0.0512
_refine_ls_wR_factor_ref         0.1564
_refine_ls_wR_factor_gt          0.1307
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_restrained_S_all      1.022
_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
Ni1 Ni 0.23535(2) 0.11815(3) 0.79360(2) 0.03433(10) Uani 1 1 d . . . . .
P1 P 0.42116(5) -0.00494(6) 0.81705(3) 0.03523(14) Uani 1 1 d . . . . .
Na1 Na -0.04996(11) 0.41263(11) 0.80625(7) 0.0718(4) Uani 1 1 d D . . . .
O1 O 0.08589(17) 0.23545(18) 0.76041(11) 0.0567(5) Uani 1 1 d D . . . .
H1O H 0.070(3) 0.192(2) 0.7351(15) 0.068 Uiso 1 1 d D U . . .
O2 O 0.13921(19) 0.5082(2) 1.07457(13) 0.0714(6) Uani 1 1 d . . . . .
N1 N 0.25024(15) -0.01857(18) 0.73637(9) 0.0343(4) Uani 1 1 d . . . . .
C1 C 0.4635(2) -0.1292(2) 0.75863(13) 0.0414(6) Uani 1 1 d . . . . .
H1 H 0.545205 -0.194548 0.750651 0.050 Uiso 1 1 calc R U . . .
C2 C 0.36496(19) -0.1205(2) 0.72608(11) 0.0356(5) Uani 1 1 d . . . . .
C3 C 0.3855(2) -0.2274(2) 0.68192(14) 0.0459(6) Uani 1 1 d . . . . .
C4 C 0.3084(3) -0.2921(3) 0.7060(2) 0.0735(9) Uani 1 1 d . . . . .
H4 H 0.238764 -0.265778 0.748089 0.088 Uiso 1 1 calc R U . . .
C5 C 0.3336(5) -0.3946(4) 0.6683(3) 0.1090(15) Uani 1 1 d . . . . .
H5 H 0.281875 -0.437818 0.685901 0.131 Uiso 1 1 calc R U . . .
C6 C 0.4339(6) -0.4340(4) 0.6054(3) 0.1144(16) Uani 1 1 d . . . . .
H6 H 0.449534 -0.503112 0.580035 0.137 Uiso 1 1 calc R U . . .
C7 C 0.5122(4) -0.3706(4) 0.5795(2) 0.1014(14) Uani 1 1 d . . . . .
H7 H 0.580129 -0.396777 0.536482 0.122 Uiso 1 1 calc R U . . .
C8 C 0.4891(3) -0.2675(3) 0.61802(16) 0.0685(8) Uani 1 1 d . . . . .
H8 H 0.542404 -0.225674 0.601271 0.082 Uiso 1 1 calc R U . . .
C9 C 0.4310(2) -0.0694(2) 0.91563(13) 0.0439(6) Uani 1 1 d . . . . .
H9 H 0.409069 -0.002318 0.949275 0.053 Uiso 1 1 calc R U . . .
C10 C 0.3300(3) -0.1222(3) 0.94330(16) 0.0629(8) Uani 1 1 d . . . . .
H10A H 0.350294 -0.188850 0.911415 0.094 Uiso 1 1 calc R U . . .
H10B H 0.245054 -0.059927 0.940624 0.094 Uiso 1 1 calc R U . . .
H10C H 0.330726 -0.151335 0.995391 0.094 Uiso 1 1 calc R U . . .
C11 C 0.5681(3) -0.1667(3) 0.92087(16) 0.0665(9) Uani 1 1 d . . . . .
H11A H 0.566233 -0.200861 0.972037 0.100 Uiso 1 1 calc R U . . .
H11B H 0.629103 -0.129508 0.908476 0.100 Uiso 1 1 calc R U . . .
H11C H 0.594306 -0.230378 0.885346 0.100 Uiso 1 1 calc R U . . .
C12 C 0.5555(2) 0.0464(3) 0.78811(14) 0.0486(6) Uani 1 1 d . . . . .
H12 H 0.637774 -0.027042 0.782170 0.058 Uiso 1 1 calc R U . . .
C13 C 0.5503(3) 0.1105(3) 0.70984(16) 0.0692(9) Uani 1 1 d . . . . .
H13A H 0.473049 0.185626 0.714208 0.104 Uiso 1 1 calc R U . . .
H13B H 0.548482 0.058464 0.674464 0.104 Uiso 1 1 calc R U . . .
H13C H 0.626066 0.127877 0.691479 0.104 Uiso 1 1 calc R U . . .
C14 C 0.5572(3) 0.1263(3) 0.84690(17) 0.0605(7) Uani 1 1 d . . . . .
H14A H 0.625919 0.153321 0.826818 0.091 Uiso 1 1 calc R U . . .
H14B H 0.572002 0.079646 0.893509 0.091 Uiso 1 1 calc R U . . .
H14C H 0.474862 0.196063 0.857253 0.091 Uiso 1 1 calc R U . . .
C15 C 0.15130(19) -0.0045(2) 0.69763(12) 0.0373(5) Uani 1 1 d . . . . .
C16 C 0.1636(2) 0.0281(2) 0.61936(12) 0.0425(6) Uani 1 1 d . . . . .
C17 C 0.0597(2) 0.0498(3) 0.58527(14) 0.0585(8) Uani 1 1 d . . . . .
H17 H 0.066953 0.071100 0.533382 0.070 Uiso 1 1 calc R U . . .
C18 C -0.0532(2) 0.0403(3) 0.62667(17) 0.0667(9) Uani 1 1 d . . . . .
H18 H -0.121419 0.055783 0.603008 0.080 Uiso 1 1 calc R U . . .
C19 C -0.0639(2) 0.0080(3) 0.70309(16) 0.0615(8) Uani 1 1 d . . . . .
H19 H -0.139857 0.001044 0.730639 0.074 Uiso 1 1 calc R U . . .
C20 C 0.0356(2) -0.0149(3) 0.74065(14) 0.0483(6) Uani 1 1 d . . . . .
C21 C 0.2830(2) 0.0472(3) 0.57317(13) 0.0512(7) Uani 1 1 d . . . . .
H21 H 0.353405 0.004664 0.600873 0.061 Uiso 1 1 calc R U . . .
C22 C 0.2560(3) 0.1832(3) 0.56840(19) 0.0788(10) Uani 1 1 d . . . . .
H22A H 0.186405 0.227795 0.542103 0.118 Uiso 1 1 calc R U . . .
H22B H 0.333356 0.193245 0.540868 0.118 Uiso 1 1 calc R U . . .
H22C H 0.231337 0.213856 0.619251 0.118 Uiso 1 1 calc R U . . .
C23 C 0.3310(3) -0.0071(3) 0.49328(15) 0.0764(10) Uani 1 1 d . . . . .
H23A H 0.345961 -0.091917 0.497794 0.115 Uiso 1 1 calc R U . . .
H23B H 0.411036 0.000097 0.468424 0.115 Uiso 1 1 calc R U . . .
H23C H 0.266306 0.036254 0.463453 0.115 Uiso 1 1 calc R U . . .
C24 C 0.0200(3) -0.0480(3) 0.82525(15) 0.0672(9) Uani 1 1 d . . . . .
H24 H 0.107673 -0.088819 0.835877 0.081 Uiso 1 1 calc R U . . .
C25 C -0.0558(3) 0.0647(4) 0.87593(17) 0.0967(13) Uani 1 1 d . . . . .
H25A H -0.009187 0.116183 0.865767 0.145 Uiso 1 1 calc R U . . .
H25B H -0.064730 0.039089 0.928946 0.145 Uiso 1 1 calc R U . . .
H25C H -0.140776 0.109529 0.864774 0.145 Uiso 1 1 calc R U . . .
C26 C -0.0452(4) -0.1379(4) 0.8484(2) 0.1063(15) Uani 1 1 d . . . . .
H26A H -0.130806 -0.101315 0.837476 0.159 Uiso 1 1 calc R U . . .
H26B H -0.052014 -0.157109 0.902239 0.159 Uiso 1 1 calc R U . . .
H26C H 0.006626 -0.211510 0.819826 0.159 Uiso 1 1 calc R U . . .
C27 C 0.21972(19) 0.2407(2) 0.85628(12) 0.0365(5) Uani 1 1 d . . . . .
C28 C 0.2267(2) 0.3513(2) 0.82691(14) 0.0494(6) Uani 1 1 d . . . . .
H28 H 0.243494 0.363621 0.773973 0.059 Uiso 1 1 calc R U . . .
C29 C 0.2097(2) 0.4433(2) 0.87297(15) 0.0514(6) Uani 1 1 d . . . . .
H29 H 0.216840 0.514314 0.850340 0.062 Uiso 1 1 calc R U . . .
C30 C 0.1821(2) 0.4307(2) 0.95267(14) 0.0443(6) Uani 1 1 d . . . . .
C31 C 0.1697(2) 0.3229(2) 0.98362(13) 0.0413(5) Uani 1 1 d . . . . .
H31 H 0.148277 0.312784 1.036606 0.050 Uiso 1 1 calc R U . . .
C32 C 0.1885(2) 0.2316(2) 0.93735(12) 0.0392(5) Uani 1 1 d . . . . .
H32 H 0.180383 0.161160 0.960269 0.047 Uiso 1 1 calc R U . . .
C33 C 0.1658(2) 0.5235(3) 1.00552(19) 0.0577(7) Uani 1 1 d . . . . .
C34 C 0.1834(4) 0.6382(3) 0.9736(2) 0.0901(11) Uani 1 1 d . . . . .
H34A H 0.165620 0.690014 1.014984 0.135 Uiso 1 1 calc R U . . .
H34B H 0.124144 0.680900 0.940315 0.135 Uiso 1 1 calc R U . . .
H34C H 0.271541 0.616745 0.945100 0.135 Uiso 1 1 calc R U . . .
O3A O -0.0326(10) 0.5641(5) 0.7157(4) 0.1109(16) Uani 0.682(7) 1 d D U P A 1
C35A C 0.0396(9) 0.5413(7) 0.6386(5) 0.139(2) Uani 0.682(7) 1 d D U P A 1
H35A H 0.041346 0.468105 0.620717 0.166 Uiso 0.682(7) 1 calc R U P A 1
H35B H 0.128743 0.530170 0.634813 0.166 Uiso 0.682(7) 1 calc R U P A 1
C36A C -0.0273(9) 0.6488(7) 0.5929(3) 0.158(2) Uani 0.682(7) 1 d D U P A 1
H36A H 0.029992 0.688986 0.569198 0.190 Uiso 0.682(7) 1 calc R U P A 1
H36B H -0.054225 0.625102 0.552842 0.190 Uiso 0.682(7) 1 calc R U P A 1
C37A C -0.1413(8) 0.7305(7) 0.6466(4) 0.140(2) Uani 0.682(7) 1 d D U P A 1
H37A H -0.134145 0.807016 0.648820 0.169 Uiso 0.682(7) 1 calc R U P A 1
H37B H -0.220083 0.748497 0.628927 0.169 Uiso 0.682(7) 1 calc R U P A 1
C38A C -0.1489(7) 0.6763(6) 0.7180(3) 0.125(2) Uani 0.682(7) 1 d D U P A 1
H38A H -0.225901 0.658850 0.732167 0.150 Uiso 0.682(7) 1 calc R U P A 1
H38B H -0.154992 0.730368 0.755601 0.150 Uiso 0.682(7) 1 calc R U P A 1
O3B O -0.019(2) 0.5562(11) 0.7113(10) 0.117(3) Uani 0.318(7) 1 d D U P A 2
C35B C 0.065(2) 0.5052(9) 0.6388(10) 0.130(3) Uani 0.318(7) 1 d D U P A 2
H35C H 0.036594 0.450863 0.620623 0.157 Uiso 0.318(7) 1 calc R U P A 2
H35D H 0.154060 0.458679 0.644928 0.157 Uiso 0.318(7) 1 calc R U P A 2
C36B C 0.0582(18) 0.6080(12) 0.5832(6) 0.143(3) Uani 0.318(7) 1 d D U P A 2
H36C H 0.028611 0.599862 0.539171 0.172 Uiso 0.318(7) 1 calc R U P A 2
H36D H 0.143092 0.610725 0.565589 0.172 Uiso 0.318(7) 1 calc R U P A 2
C37B C -0.0369(19) 0.7194(12) 0.6261(10) 0.133(3) Uani 0.318(7) 1 d D U P A 2
H37C H 0.000842 0.778497 0.620997 0.160 Uiso 0.318(7) 1 calc R U P A 2
H37D H -0.114868 0.756358 0.605240 0.160 Uiso 0.318(7) 1 calc R U P A 2
C38B C -0.0687(18) 0.6882(11) 0.7022(7) 0.127(3) Uani 0.318(7) 1 d D U P A 2
H38C H -0.162763 0.724569 0.720417 0.152 Uiso 0.318(7) 1 calc R U P A 2
H38D H -0.030896 0.719319 0.732352 0.152 Uiso 0.318(7) 1 calc R U P A 2
O4A O -0.2555(6) 0.4381(17) 0.7863(7) 0.162(2) Uani 0.541(8) 1 d D U P A 1
C39A C -0.3815(10) 0.5117(11) 0.8344(7) 0.169(3) Uani 0.541(8) 1 d D U P A 1
H39A H -0.442274 0.555704 0.801402 0.202 Uiso 0.541(8) 1 calc R U P A 1
H39B H -0.371034 0.571981 0.859629 0.202 Uiso 0.541(8) 1 calc R U P A 1
C40A C -0.4405(12) 0.4429(13) 0.8938(8) 0.194(4) Uani 0.541(8) 1 d D U P A 1
H40A H -0.527838 0.462924 0.889047 0.291 Uiso 0.541(8) 1 calc R U P A 1
H40B H -0.442679 0.464601 0.943792 0.291 Uiso 0.541(8) 1 calc R U P A 1
H40C H -0.389175 0.356674 0.887120 0.291 Uiso 0.541(8) 1 calc R U P A 1
C41A C -0.3314(11) 0.4158(14) 0.7410(7) 0.185(3) Uani 0.541(8) 1 d D U P A 1
H41A H -0.396777 0.491142 0.724980 0.222 Uiso 0.541(8) 1 calc R U P A 1
H41B H -0.372264 0.362534 0.767744 0.222 Uiso 0.541(8) 1 calc R U P A 1
C42A C -0.2230(17) 0.3550(18) 0.6766(9) 0.214(5) Uani 0.541(8) 1 d D U P A 1
H42A H -0.161547 0.280382 0.694785 0.321 Uiso 0.541(8) 1 calc R U P A 1
H42B H -0.180356 0.408032 0.654819 0.321 Uiso 0.541(8) 1 calc R U P A 1
H42C H -0.256449 0.336800 0.638235 0.321 Uiso 0.541(8) 1 calc R U P A 1
O4B O -0.2527(7) 0.449(2) 0.7806(9) 0.160(2) Uani 0.459(8) 1 d D U P A 2
C39B C -0.3622(13) 0.4729(19) 0.8463(8) 0.175(3) Uani 0.459(8) 1 d D U P A 2
H39C H -0.391035 0.553269 0.866607 0.210 Uiso 0.459(8) 1 calc R U P A 2
H39D H -0.340533 0.411452 0.886738 0.210 Uiso 0.459(8) 1 calc R U P A 2
C40B C -0.4611(12) 0.4659(15) 0.8113(10) 0.188(4) Uani 0.459(8) 1 d D U P A 2
H40D H -0.418539 0.407866 0.770834 0.283 Uiso 0.459(8) 1 calc R U P A 2
H40E H -0.509604 0.544969 0.790765 0.283 Uiso 0.459(8) 1 calc R U P A 2
H40F H -0.519586 0.440479 0.849607 0.283 Uiso 0.459(8) 1 calc R U P A 2
C41B C -0.2567(15) 0.3666(14) 0.7307(8) 0.166(3) Uani 0.459(8) 1 d D U P A 2
H41C H -0.346218 0.384572 0.729728 0.199 Uiso 0.459(8) 1 calc R U P A 2
H41D H -0.214954 0.282238 0.747643 0.199 Uiso 0.459(8) 1 calc R U P A 2
C42B C -0.1846(18) 0.3884(17) 0.6539(8) 0.170(4) Uani 0.459(8) 1 d D U P A 2
H42D H -0.198486 0.472857 0.648231 0.254 Uiso 0.459(8) 1 calc R U P A 2
H42E H -0.215663 0.368466 0.614970 0.254 Uiso 0.459(8) 1 calc R U P A 2
H42F H -0.093033 0.337832 0.648760 0.254 Uiso 0.459(8) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 1.8916(18) . ?
Ni1 C27 1.896(3) . ?
Ni1 N1 1.981(2) . ?
Ni1 P1 2.1438(12) . ?
P1 C1 1.765(3) . ?
P1 C12 1.851(3) . ?
P1 C9 1.857(3) . ?
Na1 O1 2.160(2) . ?
Na1 O2 2.271(3) 2_567 ?
Na1 O3A 2.335(4) . ?
Na1 O3B 2.353(5) . ?
Na1 O4B 2.357(5) . ?
Na1 O4A 2.384(4) . ?
Na1 C28 3.080(3) . ?
O1 H1O 0.841(9) . ?
O2 C33 1.214(4) . ?
N1 C2 1.363(3) . ?
N1 C15 1.427(3) . ?
C1 C2 1.370(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.504(3) . ?
C3 C4 1.385(4) . ?
C3 C8 1.399(4) . ?
C4 C5 1.373(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.367(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.388(6) . ?
C6 H6 0.9300 . ?
C7 C8 1.395(5) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C10 1.516(4) . ?
C9 C11 1.539(3) . ?
C9 H9 0.9800 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.522(4) . ?
C12 C14 1.530(4) . ?
C12 H12 0.9800 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.403(3) . ?
C15 C20 1.420(3) . ?
C16 C17 1.399(3) . ?
C16 C21 1.521(3) . ?
C17 C18 1.380(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.372(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.392(3) . ?
C19 H19 0.9300 . ?
C20 C24 1.511(4) . ?
C21 C23 1.529(4) . ?
C21 C22 1.532(4) . ?
C21 H21 0.9800 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 C25 1.534(5) . ?
C24 C26 1.535(5) . ?
C24 H24 0.9800 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C28 1.402(4) . ?
C27 C32 1.415(3) . ?
C28 C29 1.389(4) . ?
C28 H28 0.9300 . ?
C29 C30 1.394(4) . ?
C29 H29 0.9300 . ?
C30 C31 1.402(4) . ?
C30 C33 1.483(4) . ?
C31 C32 1.377(3) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 C34 1.510(5) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
O3A C35A 1.422(4) . ?
O3A C38A 1.444(5) . ?
C35A C36A 1.470(5) . ?
C35A H35A 0.9700 . ?
C35A H35B 0.9700 . ?
C36A C37A 1.465(5) . ?
C36A H36A 0.9700 . ?
C36A H36B 0.9700 . ?
C37A C38A 1.368(9) . ?
C37A H37A 0.9700 . ?
C37A H37B 0.9700 . ?
C38A H38A 0.9700 . ?
C38A H38B 0.9700 . ?
O3B C35B 1.445(5) . ?
O3B C38B 1.450(5) . ?
C35B C36B 1.482(5) . ?
C35B H35C 0.9700 . ?
C35B H35D 0.9700 . ?
C36B C37B 1.482(5) . ?
C36B H36C 0.9700 . ?
C36B H36D 0.9700 . ?
C37B C38B 1.375(17) . ?
C37B H37C 0.9700 . ?
C37B H37D 0.9700 . ?
C38B H38C 0.9700 . ?
C38B H38D 0.9700 . ?
O4A C39A 1.460(5) . ?
O4A C41A 1.460(5) . ?
C39A C40A 1.484(5) . ?
C39A C41A 1.984(15) . ?
C39A H39A 0.9700 . ?
C39A H39B 0.9700 . ?
C40A H40A 0.9600 . ?
C40A H40B 0.9600 . ?
C40A H40C 0.9600 . ?
C41A C42A 1.470(5) . ?
C41A H41A 0.9700 . ?
C41A H41B 0.9700 . ?
C42A H42A 0.9600 . ?
C42A H42B 0.9600 . ?
C42A H42C 0.9600 . ?
O4B C41B 1.441(5) . ?
O4B C39B 1.455(5) . ?
C39B C40B 1.476(5) . ?
C39B H39C 0.9700 . ?
C39B H39D 0.9700 . ?
C40B H40D 0.9600 . ?
C40B H40E 0.9600 . ?
C40B H40F 0.9600 . ?
C41B C42B 1.484(5) . ?
C41B H41C 0.9700 . ?
C41B H41D 0.9700 . ?
C42B H42D 0.9600 . ?
C42B H42E 0.9600 . ?
C42B H42F 0.9600 . ?

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 Ni1 C27 87.41(9) . . ?
O1 Ni1 N1 95.17(8) . . ?
C27 Ni1 N1 175.01(9) . . ?
O1 Ni1 P1 171.42(7) . . ?
C27 Ni1 P1 92.59(7) . . ?
N1 Ni1 P1 85.49(6) . . ?
C1 P1 C12 106.83(11) . . ?
C1 P1 C9 106.37(12) . . ?
C12 P1 C9 104.36(11) . . ?
C1 P1 Ni1 101.54(8) . . ?
C12 P1 Ni1 117.17(10) . . ?
C9 P1 Ni1 119.47(8) . . ?
O1 Na1 O2 135.26(10) . 2_567 ?
O1 Na1 O3A 109.0(2) . . ?
O2 Na1 O3A 110.5(2) 2_567 . ?
O1 Na1 O3B 105.6(4) . . ?
O2 Na1 O3B 113.2(5) 2_567 . ?
O1 Na1 O4B 106.3(4) . . ?
O2 Na1 O4B 94.0(3) 2_567 . ?
O3B Na1 O4B 92.1(9) . . ?
O1 Na1 O4A 104.8(4) . . ?
O2 Na1 O4A 92.8(3) 2_567 . ?
O3A Na1 O4A 93.7(6) . . ?
O1 Na1 C28 69.18(8) . . ?
O2 Na1 C28 91.03(9) 2_567 . ?
O3A Na1 C28 89.3(3) . . ?
O3B Na1 C28 86.9(7) . . ?
O4B Na1 C28 174.9(3) . . ?
O4A Na1 C28 173.9(4) . . ?
Ni1 O1 Na1 129.51(10) . . ?
Ni1 O1 H1O 101(2) . . ?
Na1 O1 H1O 126(2) . . ?
C33 O2 Na1 149.7(2) . 2_567 ?
C2 N1 C15 120.32(19) . . ?
C2 N1 Ni1 118.18(14) . . ?
C15 N1 Ni1 120.91(15) . . ?
C2 C1 P1 113.87(16) . . ?
C2 C1 H1 123.1 . . ?
P1 C1 H1 123.1 . . ?
N1 C2 C1 120.0(2) . . ?
N1 C2 C3 121.63(19) . . ?
C1 C2 C3 118.30(19) . . ?
C4 C3 C8 118.9(3) . . ?
C4 C3 C2 121.2(2) . . ?
C8 C3 C2 119.8(3) . . ?
C5 C4 C3 120.8(4) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C6 C5 C4 120.8(4) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C7 119.8(4) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 H6 120.1 . . ?
C6 C7 C8 120.0(4) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C3 119.8(4) . . ?
C7 C8 H8 120.1 . . ?
C3 C8 H8 120.1 . . ?
C10 C9 C11 110.6(2) . . ?
C10 C9 P1 108.85(17) . . ?
C11 C9 P1 112.93(17) . . ?
C10 C9 H9 108.1 . . ?
C11 C9 H9 108.1 . . ?
P1 C9 H9 108.1 . . ?
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 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 C14 111.5(3) . . ?
C13 C12 P1 109.05(17) . . ?
C14 C12 P1 114.13(17) . . ?
C13 C12 H12 107.3 . . ?
C14 C12 H12 107.3 . . ?
P1 C12 H12 107.3 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C20 120.30(19) . . ?
C16 C15 N1 120.53(19) . . ?
C20 C15 N1 119.00(19) . . ?
C17 C16 C15 118.4(2) . . ?
C17 C16 C21 120.2(2) . . ?
C15 C16 C21 121.29(19) . . ?
C18 C17 C16 121.7(2) . . ?
C18 C17 H17 119.2 . . ?
C16 C17 H17 119.2 . . ?
C19 C18 C17 119.3(2) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C18 C19 C20 122.0(2) . . ?
C18 C19 H19 119.0 . . ?
C20 C19 H19 119.0 . . ?
C19 C20 C15 118.3(2) . . ?
C19 C20 C24 120.8(2) . . ?
C15 C20 C24 121.0(2) . . ?
C16 C21 C23 112.7(2) . . ?
C16 C21 C22 110.6(2) . . ?
C23 C21 C22 111.1(3) . . ?
C16 C21 H21 107.4 . . ?
C23 C21 H21 107.4 . . ?
C22 C21 H21 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 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C20 C24 C25 112.5(3) . . ?
C20 C24 C26 112.4(3) . . ?
C25 C24 C26 109.5(3) . . ?
C20 C24 H24 107.4 . . ?
C25 C24 H24 107.4 . . ?
C26 C24 H24 107.4 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C32 114.6(2) . . ?
C28 C27 Ni1 123.21(18) . . ?
C32 C27 Ni1 121.93(19) . . ?
C29 C28 C27 123.3(2) . . ?
C29 C28 Na1 104.36(16) . . ?
C27 C28 Na1 82.34(14) . . ?
C29 C28 H28 118.4 . . ?
C27 C28 H28 118.4 . . ?
Na1 C28 H28 83.1 . . ?
C28 C29 C30 120.8(2) . . ?
C28 C29 H29 119.6 . . ?
C30 C29 H29 119.6 . . ?
C29 C30 C31 117.1(2) . . ?
C29 C30 C33 123.9(3) . . ?
C31 C30 C33 119.0(2) . . ?
C32 C31 C30 121.5(2) . . ?
C32 C31 H31 119.3 . . ?
C30 C31 H31 119.3 . . ?
C31 C32 C27 122.6(2) . . ?
C31 C32 H32 118.7 . . ?
C27 C32 H32 118.7 . . ?
O2 C33 C30 120.8(3) . . ?
O2 C33 C34 119.2(3) . . ?
C30 C33 C34 120.0(3) . . ?
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 . . ?
C35A O3A C38A 109.3(4) . . ?
C35A O3A Na1 124.5(5) . . ?
C38A O3A Na1 116.2(5) . . ?
O3A C35A C36A 106.4(4) . . ?
O3A C35A H35A 110.5 . . ?
C36A C35A H35A 110.5 . . ?
O3A C35A H35B 110.5 . . ?
C36A C35A H35B 110.5 . . ?
H35A C35A H35B 108.6 . . ?
C37A C36A C35A 106.0(4) . . ?
C37A C36A H36A 110.5 . . ?
C35A C36A H36A 110.5 . . ?
C37A C36A H36B 110.5 . . ?
C35A C36A H36B 110.5 . . ?
H36A C36A H36B 108.7 . . ?
C38A C37A C36A 109.8(5) . . ?
C38A C37A H37A 109.7 . . ?
C36A C37A H37A 109.7 . . ?
C38A C37A H37B 109.7 . . ?
C36A C37A H37B 109.7 . . ?
H37A C37A H37B 108.2 . . ?
C37A C38A O3A 108.0(4) . . ?
C37A C38A H38A 110.1 . . ?
O3A C38A H38A 110.1 . . ?
C37A C38A H38B 110.1 . . ?
O3A C38A H38B 110.1 . . ?
H38A C38A H38B 108.4 . . ?
C35B O3B C38B 107.1(5) . . ?
C35B O3B Na1 115.3(9) . . ?
C38B O3B Na1 137.5(9) . . ?
O3B C35B C36B 107.9(4) . . ?
O3B C35B H35C 110.1 . . ?
C36B C35B H35C 110.1 . . ?
O3B C35B H35D 110.1 . . ?
C36B C35B H35D 110.1 . . ?
H35C C35B H35D 108.4 . . ?
C35B C36B C37B 105.0(8) . . ?
C35B C36B H36C 110.7 . . ?
C37B C36B H36C 110.7 . . ?
C35B C36B H36D 110.7 . . ?
C37B C36B H36D 110.7 . . ?
H36C C36B H36D 108.8 . . ?
C38B C37B C36B 109.2(10) . . ?
C38B C37B H37C 109.8 . . ?
C36B C37B H37C 109.8 . . ?
C38B C37B H37D 109.8 . . ?
C36B C37B H37D 109.8 . . ?
H37C C37B H37D 108.3 . . ?
C37B C38B O3B 109.7(6) . . ?
C37B C38B H38C 109.7 . . ?
O3B C38B H38C 109.7 . . ?
C37B C38B H38D 109.7 . . ?
O3B C38B H38D 109.7 . . ?
H38C C38B H38D 108.2 . . ?
C39A O4A C41A 85.6(8) . . ?
C39A O4A Na1 124.3(7) . . ?
C41A O4A Na1 150.0(8) . . ?
O4A C39A C40A 115.7(10) . . ?
O4A C39A C41A 47.2(4) . . ?
C40A C39A C41A 102.5(11) . . ?
O4A C39A H39A 108.4 . . ?
C40A C39A H39A 108.4 . . ?
C41A C39A H39A 70.7 . . ?
O4A C39A H39B 108.4 . . ?
C40A C39A H39B 108.4 . . ?
C41A C39A H39B 147.6 . . ?
H39A C39A H39B 107.4 . . ?
C39A C40A H40A 109.5 . . ?
C39A C40A H40B 109.5 . . ?
H40A C40A H40B 109.5 . . ?
C39A C40A H40C 109.5 . . ?
H40A C40A H40C 109.5 . . ?
H40B C40A H40C 109.5 . . ?
O4A C41A C42A 97.6(8) . . ?
O4A C41A C39A 47.2(4) . . ?
C42A C41A C39A 143.9(9) . . ?
O4A C41A H41A 112.3 . . ?
C42A C41A H41A 112.2 . . ?
C39A C41A H41A 81.5 . . ?
O4A C41A H41B 112.3 . . ?
C42A C41A H41B 112.3 . . ?
C39A C41A H41B 92.1 . . ?
H41A C41A H41B 109.8 . . ?
C41A C42A H42A 109.5 . . ?
C41A C42A H42B 109.5 . . ?
H42A C42A H42B 109.5 . . ?
C41A C42A H42C 109.5 . . ?
H42A C42A H42C 109.5 . . ?
H42B C42A H42C 109.5 . . ?
C41B O4B C39B 108.7(11) . . ?
C41B O4B Na1 118.5(10) . . ?
C39B O4B Na1 116.6(8) . . ?
O4B C39B C40B 101.1(8) . . ?
O4B C39B H39C 111.5 . . ?
C40B C39B H39C 111.5 . . ?
O4B C39B H39D 111.5 . . ?
C40B C39B H39D 111.5 . . ?
H39C C39B H39D 109.4 . . ?
C39B C40B H40D 109.5 . . ?
C39B C40B H40E 109.5 . . ?
H40D C40B H40E 109.5 . . ?
C39B C40B H40F 109.5 . . ?
H40D C40B H40F 109.5 . . ?
H40E C40B H40F 109.5 . . ?
O4B C41B C42B 105.0(10) . . ?
O4B C41B H41C 110.7 . . ?
C42B C41B H41C 110.7 . . ?
O4B C41B H41D 110.7 . . ?
C42B C41B H41D 110.7 . . ?
H41C C41B H41D 108.8 . . ?
C41B C42B H42D 109.5 . . ?
C41B C42B H42E 109.5 . . ?
H42D C42B H42E 109.5 . . ?
C41B C42B H42F 109.5 . . ?
H42D C42B H42F 109.5 . . ?
H42E C42B H42F 109.5 . . ?

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
C27 Ni1 O1 Na1 -11.86(15) . . . . ?
N1 Ni1 O1 Na1 163.85(14) . . . . ?
C12 P1 C1 C2 -131.80(19) . . . . ?
C9 P1 C1 C2 117.17(19) . . . . ?
Ni1 P1 C1 C2 -8.5(2) . . . . ?
C15 N1 C2 C1 174.9(2) . . . . ?
Ni1 N1 C2 C1 3.6(3) . . . . ?
C15 N1 C2 C3 -7.4(3) . . . . ?
Ni1 N1 C2 C3 -178.71(16) . . . . ?
P1 C1 C2 N1 4.0(3) . . . . ?
P1 C1 C2 C3 -173.72(17) . . . . ?
N1 C2 C3 C4 -61.4(3) . . . . ?
C1 C2 C3 C4 116.3(3) . . . . ?
N1 C2 C3 C8 122.6(3) . . . . ?
C1 C2 C3 C8 -59.7(3) . . . . ?
C8 C3 C4 C5 0.6(5) . . . . ?
C2 C3 C4 C5 -175.5(3) . . . . ?
C3 C4 C5 C6 -1.2(6) . . . . ?
C4 C5 C6 C7 0.7(7) . . . . ?
C5 C6 C7 C8 0.5(7) . . . . ?
C6 C7 C8 C3 -1.1(6) . . . . ?
C4 C3 C8 C7 0.5(4) . . . . ?
C2 C3 C8 C7 176.7(3) . . . . ?
C1 P1 C9 C10 -63.58(19) . . . . ?
C12 P1 C9 C10 -176.34(18) . . . . ?
Ni1 P1 C9 C10 50.3(2) . . . . ?
C1 P1 C9 C11 59.7(2) . . . . ?
C12 P1 C9 C11 -53.1(2) . . . . ?
Ni1 P1 C9 C11 173.61(17) . . . . ?
C1 P1 C12 C13 72.0(2) . . . . ?
C9 P1 C12 C13 -175.59(19) . . . . ?
Ni1 P1 C12 C13 -41.0(2) . . . . ?
C1 P1 C12 C14 -162.57(19) . . . . ?
C9 P1 C12 C14 -50.2(2) . . . . ?
Ni1 P1 C12 C14 84.5(2) . . . . ?
C2 N1 C15 C16 -76.2(3) . . . . ?
Ni1 N1 C15 C16 94.9(2) . . . . ?
C2 N1 C15 C20 108.5(3) . . . . ?
Ni1 N1 C15 C20 -80.4(3) . . . . ?
C20 C15 C16 C17 -0.1(4) . . . . ?
N1 C15 C16 C17 -175.3(2) . . . . ?
C20 C15 C16 C21 176.3(2) . . . . ?
N1 C15 C16 C21 1.1(4) . . . . ?
C15 C16 C17 C18 0.3(4) . . . . ?
C21 C16 C17 C18 -176.1(3) . . . . ?
C16 C17 C18 C19 -0.5(5) . . . . ?
C17 C18 C19 C20 0.5(5) . . . . ?
C18 C19 C20 C15 -0.3(5) . . . . ?
C18 C19 C20 C24 178.8(3) . . . . ?
C16 C15 C20 C19 0.1(4) . . . . ?
N1 C15 C20 C19 175.4(3) . . . . ?
C16 C15 C20 C24 -179.1(3) . . . . ?
N1 C15 C20 C24 -3.8(4) . . . . ?
C17 C16 C21 C23 -45.0(4) . . . . ?
C15 C16 C21 C23 138.7(3) . . . . ?
C17 C16 C21 C22 80.0(3) . . . . ?
C15 C16 C21 C22 -96.3(3) . . . . ?
C19 C20 C24 C25 -82.7(4) . . . . ?
C15 C20 C24 C25 96.4(3) . . . . ?
C19 C20 C24 C26 41.6(4) . . . . ?
C15 C20 C24 C26 -139.3(3) . . . . ?
O1 Ni1 C27 C28 -60.7(2) . . . . ?
P1 Ni1 C27 C28 110.74(18) . . . . ?
O1 Ni1 C27 C32 113.65(18) . . . . ?
P1 Ni1 C27 C32 -74.94(17) . . . . ?
C32 C27 C28 C29 2.5(3) . . . . ?
Ni1 C27 C28 C29 177.16(18) . . . . ?
C32 C27 C28 Na1 -99.72(17) . . . . ?
Ni1 C27 C28 Na1 74.98(15) . . . . ?
C27 C28 C29 C30 -1.1(4) . . . . ?
Na1 C28 C29 C30 89.1(2) . . . . ?
C28 C29 C30 C31 -1.3(3) . . . . ?
C28 C29 C30 C33 178.5(2) . . . . ?
C29 C30 C31 C32 2.2(3) . . . . ?
C33 C30 C31 C32 -177.6(2) . . . . ?
C30 C31 C32 C27 -0.8(3) . . . . ?
C28 C27 C32 C31 -1.5(3) . . . . ?
Ni1 C27 C32 C31 -176.30(16) . . . . ?
Na1 O2 C33 C30 -154.7(3) 2_567 . . . ?
Na1 O2 C33 C34 25.8(5) 2_567 . . . ?
C29 C30 C33 O2 178.5(2) . . . . ?
C31 C30 C33 O2 -1.7(3) . . . . ?
C29 C30 C33 C34 -2.0(4) . . . . ?
C31 C30 C33 C34 177.8(2) . . . . ?
C38A O3A C35A C36A 5.7(13) . . . . ?
Na1 O3A C35A C36A 149.7(9) . . . . ?
O3A C35A C36A C37A -1.7(13) . . . . ?
C35A C36A C37A C38A -3.1(13) . . . . ?
C36A C37A C38A O3A 6.6(12) . . . . ?
C35A O3A C38A C37A -7.8(12) . . . . ?
Na1 O3A C38A C37A -155.1(7) . . . . ?
C38B O3B C35B C36B -5(3) . . . . ?
Na1 O3B C35B C36B 172.2(18) . . . . ?
O3B C35B C36B C37B -2(3) . . . . ?
C35B C36B C37B C38B 8(3) . . . . ?
C36B C37B C38B O3B -11(3) . . . . ?
C35B O3B C38B C37B 10(3) . . . . ?
Na1 O3B C38B C37B -166(2) . . . . ?
C41A O4A C39A C40A 83.3(16) . . . . ?
Na1 O4A C39A C40A -98.5(15) . . . . ?
Na1 O4A C39A C41A 178.2(19) . . . . ?
C39A O4A C41A C42A 171.1(14) . . . . ?
Na1 O4A C41A C42A -6(3) . . . . ?
Na1 O4A C41A C39A -177(3) . . . . ?
C41B O4B C39B C40B -32(2) . . . . ?
Na1 O4B C39B C40B -169.3(13) . . . . ?
C39B O4B C41B C42B 156.2(15) . . . . ?
Na1 O4B C41B C42B -67.6(17) . . . . ?

_refine_diff_density_max         0.528
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.061

####################################################################### 
# 
# 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_6b
_database_code_depnum_ccdc_archive 'CCDC 1944623'
loop_
_audit_author_name
_audit_author_address
'Eleuterio Alvarez'
; Spanish National Research Council (CSIC) 
Spain
;
_audit_update_record             
;
2019-11-19 deposited with the CCDC.	2019-11-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C41 H50 N2 Ni P Si, C F3 O3 S, C H2 Cl2'
_chemical_formula_sum            'C43 H52 Cl2 F3 N2 Ni O3 P S Si'
_chemical_formula_weight         922.59

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'
S S 0.1246 0.1234 '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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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'
'-x, -y, -z'

_cell_length_a                   10.8549(5)
_cell_length_b                   12.2040(6)
_cell_length_c                   18.5076(9)
_cell_angle_alpha                96.275(2)
_cell_angle_beta                 94.927(2)
_cell_angle_gamma                94.771(2)
_cell_volume                     2417.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    9851
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      29.92

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_F_000             964
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.662
_shelx_estimated_absorpt_T_min   0.733
_shelx_estimated_absorpt_T_max   0.907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6607
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   
;
program SADABS, Bruker (2001).
;
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
 Bruker-Nonius X8kappa APEX II CCD area detector
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_diffrn_detector_area_resol_mean 8.2
_diffrn_reflns_number            49159
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.112
_diffrn_reflns_theta_max         30.591
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             14773
_reflns_number_gt                11526
_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. 
  
 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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0718P)²+0.5225P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14773
_refine_ls_number_parameters     577
_refine_ls_number_restraints     147
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_ref         0.1268
_refine_ls_wR_factor_gt          0.1171
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.119
_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
Ni1 Ni 0.17451(2) 0.01157(2) 0.26127(2) 0.02215(6) Uani 1 1 d . . . . .
P1 P 0.11462(4) -0.02133(3) 0.14978(2) 0.02200(8) Uani 1 1 d . . . . .
Si1 Si 0.18265(5) -0.22686(4) 0.31397(3) 0.03390(11) Uani 1 1 d . . . . .
N1 N 0.07913(12) 0.14747(10) 0.25650(7) 0.0216(2) Uani 1 1 d . . . . .
N2 N 0.26107(13) 0.05364(11) 0.35880(7) 0.0262(3) Uani 1 1 d . . . . .
C1 C 0.10027(15) 0.23786(13) 0.31510(8) 0.0240(3) Uani 1 1 d . . . . .
C2 C 0.01176(17) 0.25608(14) 0.36508(9) 0.0301(3) Uani 1 1 d . . . . .
C3 C 0.0400(2) 0.34552(17) 0.41953(10) 0.0419(4) Uani 1 1 d . . . . .
H3 H -0.017797 0.360748 0.454200 0.050 Uiso 1 1 calc R U . . .
C4 C 0.1501(2) 0.41217(18) 0.42402(12) 0.0493(5) Uani 1 1 d . . . . .
H4 H 0.166136 0.473333 0.461017 0.059 Uiso 1 1 calc R U . . .
C5 C 0.2371(2) 0.39108(16) 0.37540(11) 0.0412(4) Uani 1 1 d . . . . .
H5 H 0.312909 0.437210 0.379728 0.049 Uiso 1 1 calc R U . . .
C6 C 0.21490(16) 0.30279(14) 0.32001(9) 0.0292(3) Uani 1 1 d . . . . .
C7 C -0.11153(18) 0.18562(16) 0.36229(11) 0.0367(4) Uani 1 1 d . . . . .
H7 H -0.116788 0.127355 0.319442 0.044 Uiso 1 1 calc R U . . .
C8 C -0.2225(2) 0.2532(2) 0.35315(13) 0.0483(5) Uani 1 1 d . . . . .
H8A H -0.228372 0.300839 0.398695 0.072 Uiso 1 1 calc R U . . .
H8B H -0.298628 0.203179 0.341370 0.072 Uiso 1 1 calc R U . . .
H8C H -0.211738 0.299226 0.313513 0.072 Uiso 1 1 calc R U . . .
C9 C -0.1226(2) 0.1277(2) 0.43151(15) 0.0614(7) Uani 1 1 d . . . . .
H9A H -0.109581 0.183057 0.474634 0.092 Uiso 1 1 calc R U . . .
H9B H -0.059854 0.074727 0.434615 0.092 Uiso 1 1 calc R U . . .
H9C H -0.205599 0.088378 0.429380 0.092 Uiso 1 1 calc R U . . .
C10 C 0.31032(16) 0.27837(15) 0.26580(10) 0.0336(4) Uani 1 1 d . . . . .
H10 H 0.306722 0.196057 0.254650 0.040 Uiso 1 1 calc R U . . .
C11 C 0.2817(2) 0.32490(17) 0.19343(12) 0.0428(4) Uani 1 1 d . . . . .
H11A H 0.199246 0.293637 0.171256 0.064 Uiso 1 1 calc R U . . .
H11B H 0.344215 0.305230 0.160331 0.064 Uiso 1 1 calc R U . . .
H11C H 0.283172 0.405675 0.202325 0.064 Uiso 1 1 calc R U . . .
C12 C 0.4438(2) 0.3193(2) 0.29678(15) 0.0564(6) Uani 1 1 d . . . . .
H12A H 0.454574 0.400311 0.300929 0.085 Uiso 1 1 calc R U . . .
H12B H 0.502004 0.288667 0.264052 0.085 Uiso 1 1 calc R U . . .
H12C H 0.460245 0.294954 0.345140 0.085 Uiso 1 1 calc R U . . .
C13 C -0.00190(13) 0.15426(12) 0.20174(8) 0.0224(3) Uani 1 1 d . . . . .
C14 C -0.01886(14) 0.05959(13) 0.14098(8) 0.0239(3) Uani 1 1 d . . . . .
H14A H -0.024503 0.088514 0.092985 0.029 Uiso 1 1 calc R U . . .
H14B H -0.096403 0.012505 0.144503 0.029 Uiso 1 1 calc R U . . .
C15 C -0.08331(15) 0.24511(13) 0.19229(8) 0.0258(3) Uani 1 1 d . . . . .
C16 C -0.20653(16) 0.21485(15) 0.16445(10) 0.0336(4) Uani 1 1 d . . . . .
H16 H -0.235273 0.138820 0.152463 0.040 Uiso 1 1 calc R U . . .
C17 C -0.28737(18) 0.29567(17) 0.15421(12) 0.0414(4) Uani 1 1 d . . . . .
H17 H -0.371445 0.274564 0.135924 0.050 Uiso 1 1 calc R U . . .
C18 C -0.24592(19) 0.40656(17) 0.17053(12) 0.0417(4) Uani 1 1 d . . . . .
H18 H -0.301399 0.461535 0.163498 0.050 Uiso 1 1 calc R U . . .
C19 C -0.12391(19) 0.43721(15) 0.19703(11) 0.0377(4) Uani 1 1 d . . . . .
H19 H -0.095218 0.513464 0.207482 0.045 Uiso 1 1 calc R U . . .
C20 C -0.04271(16) 0.35746(14) 0.20854(9) 0.0300(3) Uani 1 1 d . . . . .
H20 H 0.040857 0.379365 0.227563 0.036 Uiso 1 1 calc R U . . .
C21 C 0.23256(15) 0.03749(13) 0.09775(8) 0.0258(3) Uani 1 1 d . . . . .
C22 C 0.35697(16) 0.03301(15) 0.12274(10) 0.0320(3) Uani 1 1 d . . . . .
H22 H 0.377518 -0.000025 0.165816 0.038 Uiso 1 1 calc R U . . .
C23 C 0.45058(18) 0.07668(17) 0.08481(12) 0.0405(4) Uani 1 1 d . . . . .
H23 H 0.535047 0.073577 0.102091 0.049 Uiso 1 1 calc R U . . .
C24 C 0.4219(2) 0.12434(19) 0.02247(13) 0.0461(5) Uani 1 1 d . . . . .
H24 H 0.486434 0.153956 -0.003299 0.055 Uiso 1 1 calc R U . . .
C25 C 0.2996(2) 0.1294(2) -0.00285(12) 0.0482(5) Uani 1 1 d . . . . .
H25 H 0.280145 0.162546 -0.046007 0.058 Uiso 1 1 calc R U . . .
C26 C 0.20453(17) 0.08602(17) 0.03450(10) 0.0362(4) Uani 1 1 d . . . . .
H26 H 0.120356 0.089566 0.016781 0.043 Uiso 1 1 calc R U . . .
C27 C 0.05842(15) -0.15482(13) 0.09959(8) 0.0251(3) Uani 1 1 d . . . . .
C28 C 0.11201(17) -0.19922(15) 0.03830(10) 0.0335(4) Uani 1 1 d . . . . .
H28 H 0.182512 -0.160559 0.022485 0.040 Uiso 1 1 calc R U . . .
C29 C 0.0623(2) -0.29980(17) 0.00051(11) 0.0439(5) Uani 1 1 d . . . . .
H29 H 0.099565 -0.329904 -0.040898 0.053 Uiso 1 1 calc R U . . .
C30 C -0.0405(2) -0.35651(16) 0.02232(12) 0.0444(5) Uani 1 1 d . . . . .
H30 H -0.075423 -0.424247 -0.004713 0.053 Uiso 1 1 calc R U . . .
C31 C -0.09279(19) -0.31391(15) 0.08424(12) 0.0400(4) Uani 1 1 d . . . . .
H31 H -0.162403 -0.353686 0.100191 0.048 Uiso 1 1 calc R U . . .
C32 C -0.04372(16) -0.21352(15) 0.12283(10) 0.0325(3) Uani 1 1 d . . . . .
H32 H -0.079764 -0.184846 0.165080 0.039 Uiso 1 1 calc R U . . .
C33 C 0.24968(16) -0.12850(14) 0.25380(9) 0.0299(3) Uani 1 1 d . . . . .
H33A H 0.236972 -0.163227 0.202494 0.036 Uiso 1 1 calc R U . . .
H33B H 0.340238 -0.113864 0.267423 0.036 Uiso 1 1 calc R U . . .
C34 C 0.0249(2) -0.1979(2) 0.34065(15) 0.0569(6) Uani 1 1 d . . . . .
H34A H 0.030021 -0.124740 0.368997 0.085 Uiso 1 1 calc R U . . .
H34B H -0.005304 -0.254410 0.370319 0.085 Uiso 1 1 calc R U . . .
H34C H -0.032457 -0.199490 0.296604 0.085 Uiso 1 1 calc R U . . .
C35 C 0.2900(2) -0.2239(2) 0.39883(12) 0.0480(5) Uani 1 1 d . . . . .
H35A H 0.372678 -0.240202 0.385651 0.072 Uiso 1 1 calc R U . . .
H35B H 0.258188 -0.279629 0.428583 0.072 Uiso 1 1 calc R U . . .
H35C H 0.295541 -0.150384 0.426753 0.072 Uiso 1 1 calc R U . . .
C36 C 0.1717(3) -0.36937(19) 0.26400(16) 0.0644(7) Uani 1 1 d . . . . .
H36A H 0.122533 -0.371109 0.216867 0.097 Uiso 1 1 calc R U . . .
H36B H 0.131597 -0.421997 0.293050 0.097 Uiso 1 1 calc R U . . .
H36C H 0.255284 -0.389778 0.255859 0.097 Uiso 1 1 calc R U . . .
C37 C 0.19941(17) 0.06881(14) 0.41834(9) 0.0307(3) Uani 1 1 d . . . . .
H37 H 0.111224 0.059135 0.412508 0.037 Uiso 1 1 calc R U . . .
C38 C 0.2585(2) 0.09792(16) 0.48787(10) 0.0392(4) Uani 1 1 d . . . . .
H38 H 0.211779 0.107418 0.528842 0.047 Uiso 1 1 calc R U . . .
C39 C 0.3863(2) 0.11287(18) 0.49662(11) 0.0454(5) Uani 1 1 d . . . . .
H39 H 0.429297 0.132440 0.543776 0.054 Uiso 1 1 calc R U . . .
C40 C 0.45030(19) 0.09906(18) 0.43620(12) 0.0437(5) Uani 1 1 d . . . . .
H40 H 0.538421 0.110198 0.440962 0.052 Uiso 1 1 calc R U . . .
C41 C 0.38599(16) 0.06878(15) 0.36814(10) 0.0337(4) Uani 1 1 d . . . . .
H41 H 0.431422 0.058329 0.326676 0.040 Uiso 1 1 calc R U . . .
S1 S 0.67297(4) 0.91760(5) 0.26188(3) 0.03892(11) Uani 1 1 d . . . . .
O1 O 0.78370(16) 0.94182(16) 0.22852(12) 0.0680(5) Uani 1 1 d . . . . .
O2 O 0.57815(16) 0.98854(17) 0.25006(13) 0.0724(6) Uani 1 1 d . . . . .
O3 O 0.6932(2) 0.8937(2) 0.33541(11) 0.0930(8) Uani 1 1 d . . . . .
C42 C 0.6096(2) 0.7846(2) 0.21497(13) 0.0589(6) Uani 1 1 d D . . . .
F1A F 0.6964(5) 0.7130(5) 0.2251(6) 0.0809(16) Uani 0.59(2) 1 d D U P A 1
F2A F 0.5886(10) 0.7852(7) 0.14338(19) 0.0998(18) Uani 0.59(2) 1 d D U P A 1
F3A F 0.5072(5) 0.7412(6) 0.2395(4) 0.0619(12) Uani 0.59(2) 1 d D U P A 1
F1B F 0.6850(9) 0.7102(7) 0.1965(7) 0.081(2) Uani 0.41(2) 1 d D U P A 2
F2B F 0.5434(12) 0.8052(8) 0.1536(5) 0.093(2) Uani 0.41(2) 1 d D U P A 2
F3B F 0.5278(10) 0.7407(10) 0.2561(6) 0.071(2) Uani 0.41(2) 1 d D U P A 2
Cl1A Cl 0.7611(5) 0.5468(2) 0.3580(2) 0.1160(10) Uani 0.601(6) 1 d D U P B 1
Cl2A Cl 0.5602(2) 0.5861(3) 0.44415(17) 0.0970(7) Uani 0.601(6) 1 d D U P B 1
C43A C 0.6870(7) 0.6441(4) 0.4076(5) 0.0773(15) Uani 0.601(6) 1 d D U P B 1
H43A H 0.746212 0.683430 0.447601 0.093 Uiso 0.601(6) 1 calc R U P B 1
H43B H 0.659869 0.699193 0.375614 0.093 Uiso 0.601(6) 1 calc R U P B 1
Cl1B Cl 0.8291(6) 0.5535(3) 0.3778(2) 0.0953(11) Uani 0.399(6) 1 d D U P B 2
Cl2B Cl 0.5838(5) 0.5918(5) 0.4147(4) 0.1401(15) Uani 0.399(6) 1 d D U P B 2
C43B C 0.7318(7) 0.6492(6) 0.4059(8) 0.074(2) Uani 0.399(6) 1 d D U P B 2
H43C H 0.726772 0.703972 0.370374 0.089 Uiso 0.399(6) 1 calc R U P B 2
H43D H 0.767268 0.689058 0.453607 0.089 Uiso 0.399(6) 1 calc R U P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C33 1.9512(17) . ?
Ni1 N2 1.9572(13) . ?
Ni1 N1 2.0329(13) . ?
Ni1 P1 2.0943(4) . ?
P1 C21 1.8143(16) . ?
P1 C27 1.8154(16) . ?
P1 C14 1.8259(15) . ?
Si1 C35 1.869(2) . ?
Si1 C33 1.8699(18) . ?
Si1 C34 1.873(2) . ?
Si1 C36 1.868(2) . ?
N1 C13 1.298(2) . ?
N1 C1 1.4489(19) . ?
N2 C37 1.341(2) . ?
N2 C41 1.347(2) . ?
C1 C2 1.404(2) . ?
C1 C6 1.409(2) . ?
C2 C3 1.397(2) . ?
C2 C7 1.523(3) . ?
C3 C4 1.379(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.394(2) . ?
C5 H5 0.9500 . ?
C6 C10 1.527(2) . ?
C7 C8 1.523(3) . ?
C7 C9 1.538(3) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C12 1.534(3) . ?
C10 C11 1.529(3) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C15 1.490(2) . ?
C13 C14 1.510(2) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.396(2) . ?
C15 C20 1.397(2) . ?
C16 C17 1.391(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.383(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.379(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.388(2) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C26 1.391(2) . ?
C21 C22 1.397(2) . ?
C22 C23 1.387(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.372(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.378(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.391(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C32 1.395(2) . ?
C27 C28 1.396(2) . ?
C28 C29 1.387(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.377(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.391(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.389(3) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.383(2) . ?
C37 H37 0.9500 . ?
C38 C39 1.377(3) . ?
C38 H38 0.9500 . ?
C39 C40 1.369(3) . ?
C39 H39 0.9500 . ?
C40 C41 1.384(3) . ?
C40 H40 0.9500 . ?
C41 H41 0.9500 . ?
S1 O2 1.4170(19) . ?
S1 O1 1.4218(15) . ?
S1 O3 1.425(2) . ?
S1 C42 1.807(3) . ?
C42 F1B 1.309(4) . ?
C42 F3A 1.328(4) . ?
C42 F2A 1.326(4) . ?
C42 F3B 1.334(4) . ?
C42 F2B 1.350(4) . ?
C42 F1A 1.352(4) . ?
Cl1A C43A 1.716(4) . ?
Cl2A C43A 1.719(4) . ?
C43A H43A 0.9900 . ?
C43A H43B 0.9900 . ?
Cl1B C43B 1.708(5) . ?
Cl2B C43B 1.726(5) . ?
C43B H43C 0.9900 . ?
C43B H43D 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C33 Ni1 N2 90.48(6) . . ?
C33 Ni1 N1 171.73(6) . . ?
N2 Ni1 N1 97.52(5) . . ?
C33 Ni1 P1 88.30(5) . . ?
N2 Ni1 P1 168.73(4) . . ?
N1 Ni1 P1 84.26(4) . . ?
C21 P1 C27 105.73(7) . . ?
C21 P1 C14 107.44(7) . . ?
C27 P1 C14 103.48(7) . . ?
C21 P1 Ni1 109.06(5) . . ?
C27 P1 Ni1 127.05(5) . . ?
C14 P1 Ni1 102.63(5) . . ?
C35 Si1 C33 109.47(9) . . ?
C35 Si1 C34 108.62(12) . . ?
C33 Si1 C34 114.26(10) . . ?
C35 Si1 C36 107.91(12) . . ?
C33 Si1 C36 107.86(11) . . ?
C34 Si1 C36 108.56(13) . . ?
C13 N1 C1 119.15(13) . . ?
C13 N1 Ni1 120.87(10) . . ?
C1 N1 Ni1 119.98(10) . . ?
C37 N2 C41 117.62(15) . . ?
C37 N2 Ni1 121.86(12) . . ?
C41 N2 Ni1 120.52(12) . . ?
C2 C1 C6 122.70(15) . . ?
C2 C1 N1 120.92(14) . . ?
C6 C1 N1 116.35(14) . . ?
C3 C2 C1 116.84(17) . . ?
C3 C2 C7 119.24(16) . . ?
C1 C2 C7 123.91(15) . . ?
C4 C3 C2 121.39(18) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C5 120.78(18) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C4 C5 C6 120.69(19) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C1 117.54(16) . . ?
C5 C6 C10 121.30(16) . . ?
C1 C6 C10 121.15(15) . . ?
C8 C7 C2 112.30(17) . . ?
C8 C7 C9 107.77(16) . . ?
C2 C7 C9 112.04(18) . . ?
C8 C7 H7 108.2 . . ?
C2 C7 H7 108.2 . . ?
C9 C7 H7 108.2 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C12 C10 C11 109.20(17) . . ?
C12 C10 C6 113.06(17) . . ?
C11 C10 C6 112.85(15) . . ?
C12 C10 H10 107.1 . . ?
C11 C10 H10 107.1 . . ?
C6 C10 H10 107.1 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N1 C13 C15 127.15(14) . . ?
N1 C13 C14 117.47(13) . . ?
C15 C13 C14 115.37(13) . . ?
C13 C14 P1 108.11(10) . . ?
C13 C14 H14A 110.1 . . ?
P1 C14 H14A 110.1 . . ?
C13 C14 H14B 110.1 . . ?
P1 C14 H14B 110.1 . . ?
H14A C14 H14B 108.4 . . ?
C16 C15 C20 118.86(15) . . ?
C16 C15 C13 117.34(15) . . ?
C20 C15 C13 123.79(14) . . ?
C17 C16 C15 120.22(17) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C18 C17 C16 120.30(18) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C19 C18 C17 119.86(17) . . ?
C19 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?
C18 C19 C20 120.46(18) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
C19 C20 C15 120.29(16) . . ?
C19 C20 H20 119.9 . . ?
C15 C20 H20 119.9 . . ?
C26 C21 C22 118.99(15) . . ?
C26 C21 P1 123.04(13) . . ?
C22 C21 P1 117.96(12) . . ?
C23 C22 C21 120.15(17) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C24 C23 C22 120.36(18) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C25 C24 C23 120.16(18) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C24 C25 C26 120.26(19) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C21 C26 C25 120.07(18) . . ?
C21 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C32 C27 C28 119.29(15) . . ?
C32 C27 P1 118.17(12) . . ?
C28 C27 P1 122.52(13) . . ?
C29 C28 C27 119.99(17) . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C30 C29 C28 120.77(18) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
C29 C30 C31 119.55(18) . . ?
C29 C30 H30 120.2 . . ?
C31 C30 H30 120.2 . . ?
C30 C31 C32 120.33(18) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 H31 119.8 . . ?
C31 C32 C27 120.03(17) . . ?
C31 C32 H32 120.0 . . ?
C27 C32 H32 120.0 . . ?
Si1 C33 Ni1 112.32(9) . . ?
Si1 C33 H33A 109.1 . . ?
Ni1 C33 H33A 109.1 . . ?
Si1 C33 H33B 109.1 . . ?
Ni1 C33 H33B 109.1 . . ?
H33A C33 H33B 107.9 . . ?
Si1 C34 H34A 109.5 . . ?
Si1 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
Si1 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
Si1 C35 H35A 109.5 . . ?
Si1 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
Si1 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
Si1 C36 H36A 109.5 . . ?
Si1 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
Si1 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N2 C37 C38 122.92(17) . . ?
N2 C37 H37 118.5 . . ?
C38 C37 H37 118.5 . . ?
C39 C38 C37 118.81(18) . . ?
C39 C38 H38 120.6 . . ?
C37 C38 H38 120.6 . . ?
C40 C39 C38 118.85(18) . . ?
C40 C39 H39 120.6 . . ?
C38 C39 H39 120.6 . . ?
C39 C40 C41 119.66(19) . . ?
C39 C40 H40 120.2 . . ?
C41 C40 H40 120.2 . . ?
N2 C41 C40 122.12(18) . . ?
N2 C41 H41 118.9 . . ?
C40 C41 H41 118.9 . . ?
O2 S1 O1 115.70(12) . . ?
O2 S1 O3 114.22(15) . . ?
O1 S1 O3 114.21(15) . . ?
O2 S1 C42 104.56(12) . . ?
O1 S1 C42 103.95(11) . . ?
O3 S1 C42 102.00(13) . . ?
F3A C42 F2A 108.4(3) . . ?
F1B C42 F3B 108.6(4) . . ?
F1B C42 F2B 107.9(3) . . ?
F3B C42 F2B 106.2(4) . . ?
F3A C42 F1A 106.3(3) . . ?
F2A C42 F1A 106.3(3) . . ?
F1B C42 S1 119.4(5) . . ?
F3A C42 S1 115.2(4) . . ?
F2A C42 S1 113.0(3) . . ?
F3B C42 S1 107.7(6) . . ?
F2B C42 S1 106.4(4) . . ?
F1A C42 S1 107.1(4) . . ?
Cl2A C43A Cl1A 112.2(3) . . ?
Cl2A C43A H43A 109.2 . . ?
Cl1A C43A H43A 109.2 . . ?
Cl2A C43A H43B 109.2 . . ?
Cl1A C43A H43B 109.2 . . ?
H43A C43A H43B 107.9 . . ?
Cl1B C43B Cl2B 113.3(4) . . ?
Cl1B C43B H43C 108.9 . . ?
Cl2B C43B H43C 108.9 . . ?
Cl1B C43B H43D 108.9 . . ?
Cl2B C43B H43D 108.9 . . ?
H43C C43B H43D 107.7 . . ?

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
C13 N1 C1 C2 72.63(19) . . . . ?
Ni1 N1 C1 C2 -106.72(15) . . . . ?
C13 N1 C1 C6 -109.33(16) . . . . ?
Ni1 N1 C1 C6 71.32(16) . . . . ?
C6 C1 C2 C3 2.4(2) . . . . ?
N1 C1 C2 C3 -179.72(15) . . . . ?
C6 C1 C2 C7 -178.47(16) . . . . ?
N1 C1 C2 C7 -0.6(2) . . . . ?
C1 C2 C3 C4 -0.4(3) . . . . ?
C7 C2 C3 C4 -179.56(19) . . . . ?
C2 C3 C4 C5 -1.3(3) . . . . ?
C3 C4 C5 C6 0.9(3) . . . . ?
C4 C5 C6 C1 1.0(3) . . . . ?
C4 C5 C6 C10 -179.98(19) . . . . ?
C2 C1 C6 C5 -2.7(2) . . . . ?
N1 C1 C6 C5 179.30(15) . . . . ?
C2 C1 C6 C10 178.28(16) . . . . ?
N1 C1 C6 C10 0.3(2) . . . . ?
C3 C2 C7 C8 59.1(2) . . . . ?
C1 C2 C7 C8 -120.02(19) . . . . ?
C3 C2 C7 C9 -62.3(2) . . . . ?
C1 C2 C7 C9 118.5(2) . . . . ?
C5 C6 C10 C12 26.3(3) . . . . ?
C1 C6 C10 C12 -154.71(18) . . . . ?
C5 C6 C10 C11 -98.2(2) . . . . ?
C1 C6 C10 C11 80.7(2) . . . . ?
C1 N1 C13 C15 -2.7(2) . . . . ?
Ni1 N1 C13 C15 176.61(11) . . . . ?
C1 N1 C13 C14 178.54(13) . . . . ?
Ni1 N1 C13 C14 -2.11(18) . . . . ?
N1 C13 C14 P1 -16.53(17) . . . . ?
C15 C13 C14 P1 164.59(11) . . . . ?
C21 P1 C14 C13 -89.35(11) . . . . ?
C27 P1 C14 C13 159.09(10) . . . . ?
Ni1 P1 C14 C13 25.56(11) . . . . ?
N1 C13 C15 C16 -138.18(17) . . . . ?
C14 C13 C15 C16 40.6(2) . . . . ?
N1 C13 C15 C20 42.9(2) . . . . ?
C14 C13 C15 C20 -138.40(16) . . . . ?
C20 C15 C16 C17 -0.9(3) . . . . ?
C13 C15 C16 C17 -179.92(16) . . . . ?
C15 C16 C17 C18 0.9(3) . . . . ?
C16 C17 C18 C19 0.0(3) . . . . ?
C17 C18 C19 C20 -1.0(3) . . . . ?
C18 C19 C20 C15 1.0(3) . . . . ?
C16 C15 C20 C19 -0.1(3) . . . . ?
C13 C15 C20 C19 178.90(15) . . . . ?
C27 P1 C21 C26 77.62(16) . . . . ?
C14 P1 C21 C26 -32.39(17) . . . . ?
Ni1 P1 C21 C26 -142.94(14) . . . . ?
C27 P1 C21 C22 -102.13(14) . . . . ?
C14 P1 C21 C22 147.85(13) . . . . ?
Ni1 P1 C21 C22 37.30(14) . . . . ?
C26 C21 C22 C23 0.1(3) . . . . ?
P1 C21 C22 C23 179.90(15) . . . . ?
C21 C22 C23 C24 -0.1(3) . . . . ?
C22 C23 C24 C25 0.1(3) . . . . ?
C23 C24 C25 C26 -0.1(4) . . . . ?
C22 C21 C26 C25 -0.1(3) . . . . ?
P1 C21 C26 C25 -179.86(16) . . . . ?
C24 C25 C26 C21 0.1(3) . . . . ?
C21 P1 C27 C32 -172.78(13) . . . . ?
C14 P1 C27 C32 -59.96(14) . . . . ?
Ni1 P1 C27 C32 57.60(15) . . . . ?
C21 P1 C27 C28 5.98(16) . . . . ?
C14 P1 C27 C28 118.79(15) . . . . ?
Ni1 P1 C27 C28 -123.64(13) . . . . ?
C32 C27 C28 C29 1.1(3) . . . . ?
P1 C27 C28 C29 -177.65(15) . . . . ?
C27 C28 C29 C30 0.5(3) . . . . ?
C28 C29 C30 C31 -1.9(3) . . . . ?
C29 C30 C31 C32 1.6(3) . . . . ?
C30 C31 C32 C27 0.0(3) . . . . ?
C28 C27 C32 C31 -1.4(3) . . . . ?
P1 C27 C32 C31 177.43(14) . . . . ?
C35 Si1 C33 Ni1 -100.36(11) . . . . ?
C34 Si1 C33 Ni1 21.69(14) . . . . ?
C36 Si1 C33 Ni1 142.47(12) . . . . ?
C41 N2 C37 C38 -0.6(3) . . . . ?
Ni1 N2 C37 C38 179.62(13) . . . . ?
N2 C37 C38 C39 0.5(3) . . . . ?
C37 C38 C39 C40 0.4(3) . . . . ?
C38 C39 C40 C41 -1.1(3) . . . . ?
C37 N2 C41 C40 -0.1(3) . . . . ?
Ni1 N2 C41 C40 179.67(15) . . . . ?
C39 C40 C41 N2 0.9(3) . . . . ?
O2 S1 C42 F1B 159.4(6) . . . . ?
O1 S1 C42 F1B 37.7(7) . . . . ?
O3 S1 C42 F1B -81.3(7) . . . . ?
O2 S1 C42 F3A -61.4(4) . . . . ?
O1 S1 C42 F3A 176.8(4) . . . . ?
O3 S1 C42 F3A 57.8(4) . . . . ?
O2 S1 C42 F2A 63.9(6) . . . . ?
O1 S1 C42 F2A -57.9(6) . . . . ?
O3 S1 C42 F2A -176.9(6) . . . . ?
O2 S1 C42 F3B -76.3(6) . . . . ?
O1 S1 C42 F3B 161.9(6) . . . . ?
O3 S1 C42 F3B 42.9(6) . . . . ?
O2 S1 C42 F2B 37.2(7) . . . . ?
O1 S1 C42 F2B -84.6(7) . . . . ?
O3 S1 C42 F2B 156.4(7) . . . . ?
O2 S1 C42 F1A -179.5(5) . . . . ?
O1 S1 C42 F1A 58.8(5) . . . . ?
O3 S1 C42 F1A -60.2(5) . . . . ?

_refine_diff_density_max         0.684
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.066


####################################################################### 
# 
# 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_4c
_database_code_depnum_ccdc_archive 'CCDC 1944622'
loop_
_audit_author_name
_audit_author_address
'Eleuterio Alvarez'
; Spanish National Research Council (CSIC) 
Spain
;
_audit_update_record             
;
2019-11-19 deposited with the CCDC.	2019-11-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H60 N O2 P Pd Si2'
_chemical_formula_sum            'C42 H60 N O2 P Pd Si2'
_chemical_formula_weight         804.46

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   12.8081(15)
_cell_length_b                   22.863(3)
_cell_length_c                   14.9029(18)
_cell_angle_alpha                90
_cell_angle_beta                 98.384(3)
_cell_angle_gamma                90
_cell_volume                     4317.4(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    9891
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      27.85

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_F_000             1696
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.555
_shelx_estimated_absorpt_T_min   0.897
_shelx_estimated_absorpt_T_max   0.973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4598
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   
; 
program SADABS, Bruker (2001). 
;
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
; 
 Bruker-Nonius X8kappa APEX II CCD area detector 
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_diffrn_detector_area_resol_mean 8.2
_diffrn_reflns_number            62440
_diffrn_reflns_av_unetI/netI     0.0640
_diffrn_reflns_av_R_equivalents  0.0787
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.643
_diffrn_reflns_theta_max         30.658
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             12943
_reflns_number_gt                9222
_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. 
  
 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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.1040P)²+38.2542P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12943
_refine_ls_number_parameters     454
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1306
_refine_ls_R_factor_gt           0.0951
_refine_ls_wR_factor_ref         0.2801
_refine_ls_wR_factor_gt          0.2490
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_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
Pd1 Pd 0.29932(4) 0.16682(2) 0.31072(3) 0.02704(14) Uani 1 1 d . . . . .
P1 P 0.19587(12) 0.09778(7) 0.22776(10) 0.0279(3) Uani 1 1 d . . . . .
Si1 Si 0.32622(15) 0.08438(9) 0.49974(12) 0.0348(4) Uani 1 1 d . . . . .
Si2 Si 0.33776(16) 0.29292(9) 0.43663(14) 0.0369(4) Uani 1 1 d . . . . .
O1 O 0.1497(5) 0.0292(3) 0.0472(4) 0.0536(15) Uani 1 1 d . . . . .
O2 O 0.0177(4) 0.1589(2) 0.2809(4) 0.0429(12) Uani 1 1 d . . . . .
N1 N 0.3242(4) 0.1892(2) 0.1694(3) 0.0270(10) Uani 1 1 d . . . . .
C1 C 0.2520(5) 0.1723(3) 0.1038(4) 0.0283(11) Uani 1 1 d . . . . .
C2 C 0.1531(5) 0.1458(3) 0.1299(4) 0.0325(12) Uani 1 1 d . . . . .
H2A H 0.115201 0.123017 0.078763 0.039 Uiso 1 1 calc R U . . .
H2B H 0.105469 0.176829 0.146592 0.039 Uiso 1 1 calc R U . . .
C3 C 0.2563(5) 0.1771(3) 0.0057(4) 0.0311(12) Uani 1 1 d . . . . .
C4 C 0.3452(6) 0.1608(4) -0.0313(5) 0.0432(17) Uani 1 1 d . . . . .
H4 H 0.406655 0.148104 0.007322 0.052 Uiso 1 1 calc R U . . .
C5 C 0.3451(7) 0.1631(4) -0.1252(5) 0.051(2) Uani 1 1 d . . . . .
H5 H 0.405999 0.151546 -0.150250 0.062 Uiso 1 1 calc R U . . .
C6 C 0.2566(8) 0.1820(4) -0.1810(5) 0.052(2) Uani 1 1 d . . . . .
H6 H 0.256769 0.183715 -0.244655 0.062 Uiso 1 1 calc R U . . .
C7 C 0.1686(7) 0.1983(4) -0.1457(5) 0.0455(17) Uani 1 1 d . . . . .
H7 H 0.107817 0.211417 -0.184797 0.055 Uiso 1 1 calc R U . . .
C8 C 0.1677(5) 0.1957(3) -0.0538(4) 0.0373(14) Uani 1 1 d . . . . .
H8 H 0.105677 0.206683 -0.030046 0.045 Uiso 1 1 calc R U . . .
C9 C 0.4115(5) 0.2234(3) 0.1466(4) 0.0279(11) Uani 1 1 d . . . . .
C10 C 0.5131(5) 0.1988(3) 0.1592(4) 0.0345(14) Uani 1 1 d . . . . .
C11 C 0.5951(5) 0.2331(4) 0.1374(5) 0.0410(16) Uani 1 1 d . . . . .
H11 H 0.664256 0.217091 0.143890 0.049 Uiso 1 1 calc R U . . .
C12 C 0.5792(6) 0.2894(4) 0.1068(5) 0.0457(18) Uani 1 1 d . . . . .
H12 H 0.636840 0.311901 0.092344 0.055 Uiso 1 1 calc R U . . .
C13 C 0.4792(6) 0.3134(4) 0.0971(5) 0.0433(16) Uani 1 1 d . . . . .
H13 H 0.469180 0.352665 0.077027 0.052 Uiso 1 1 calc R U . . .
C14 C 0.3929(5) 0.2811(3) 0.1160(4) 0.0341(13) Uani 1 1 d . . . . .
C15 C 0.5332(5) 0.1368(4) 0.1938(5) 0.0412(16) Uani 1 1 d . . . . .
H15 H 0.463566 0.117763 0.196992 0.049 Uiso 1 1 calc R U . . .
C16 C 0.5924(9) 0.1004(5) 0.1308(6) 0.064(3) Uani 1 1 d . . . . .
H16A H 0.557255 0.104380 0.068103 0.096 Uiso 1 1 calc R U . . .
H16B H 0.592282 0.059150 0.148843 0.096 Uiso 1 1 calc R U . . .
H16C H 0.665294 0.114288 0.135139 0.096 Uiso 1 1 calc R U . . .
C17 C 0.5973(8) 0.1367(5) 0.2895(6) 0.058(2) Uani 1 1 d . . . . .
H17A H 0.667951 0.152428 0.286848 0.087 Uiso 1 1 calc R U . . .
H17B H 0.603165 0.096600 0.312806 0.087 Uiso 1 1 calc R U . . .
H17C H 0.561530 0.161078 0.329795 0.087 Uiso 1 1 calc R U . . .
C18 C 0.2849(6) 0.3102(3) 0.1021(5) 0.0384(14) Uani 1 1 d . . . . .
H18 H 0.230684 0.279704 0.108688 0.046 Uiso 1 1 calc R U . . .
C19 C 0.2778(9) 0.3572(5) 0.1730(7) 0.065(3) Uani 1 1 d . . . . .
H19A H 0.287911 0.339428 0.233493 0.098 Uiso 1 1 calc R U . . .
H19B H 0.208242 0.375866 0.161721 0.098 Uiso 1 1 calc R U . . .
H19C H 0.332697 0.386667 0.169613 0.098 Uiso 1 1 calc R U . . .
C20 C 0.2588(7) 0.3374(4) 0.0072(6) 0.0504(19) Uani 1 1 d . . . . .
H20A H 0.304410 0.371357 0.002497 0.076 Uiso 1 1 calc R U . . .
H20B H 0.184786 0.349798 -0.002881 0.076 Uiso 1 1 calc R U . . .
H20C H 0.270587 0.308369 -0.038707 0.076 Uiso 1 1 calc R U . . .
C21 C 0.2690(5) 0.0390(3) 0.1826(4) 0.0319(12) Uani 1 1 d . . . . .
C22 C 0.2445(6) 0.0139(3) 0.0954(5) 0.0401(15) Uani 1 1 d . . . . .
C23 C 0.3149(7) -0.0241(4) 0.0633(6) 0.0507(19) Uani 1 1 d . . . . .
H23 H 0.299931 -0.038922 0.003241 0.061 Uiso 1 1 calc R U . . .
C24 C 0.4064(7) -0.0405(4) 0.1180(7) 0.059(2) Uani 1 1 d . . . . .
H24 H 0.454528 -0.066433 0.095617 0.071 Uiso 1 1 calc R U . . .
C25 C 0.4280(7) -0.0189(4) 0.2060(7) 0.058(2) Uani 1 1 d . . . . .
H25 H 0.488326 -0.032311 0.245419 0.069 Uiso 1 1 calc R U . . .
C26 C 0.3622(6) 0.0216(3) 0.2358(5) 0.0436(16) Uani 1 1 d . . . . .
H26 H 0.380680 0.038286 0.294315 0.052 Uiso 1 1 calc R U . . .
C27 C 0.1326(9) 0.0164(5) -0.0472(6) 0.065(3) Uani 1 1 d . . . . .
H27A H 0.184416 0.037607 -0.077186 0.097 Uiso 1 1 calc R U . . .
H27B H 0.061251 0.028645 -0.073234 0.097 Uiso 1 1 calc R U . . .
H27C H 0.140417 -0.025698 -0.056250 0.097 Uiso 1 1 calc R U . . .
C28 C 0.0737(5) 0.0643(3) 0.2535(4) 0.0354(13) Uani 1 1 d . . . . .
C29 C -0.0018(5) 0.1009(4) 0.2816(5) 0.0396(15) Uani 1 1 d . . . . .
C30 C -0.0911(7) 0.0761(5) 0.3094(7) 0.060(2) Uani 1 1 d . . . . .
H30 H -0.142927 0.100397 0.329908 0.072 Uiso 1 1 calc R U . . .
C31 C -0.1040(8) 0.0166(5) 0.3073(8) 0.071(3) Uani 1 1 d . . . . .
H31 H -0.165660 0.000366 0.325829 0.085 Uiso 1 1 calc R U . . .
C32 C -0.0313(7) -0.0198(4) 0.2795(7) 0.059(2) Uani 1 1 d . . . . .
H32 H -0.041583 -0.060914 0.279200 0.070 Uiso 1 1 calc R U . . .
C33 C 0.0586(6) 0.0041(4) 0.2515(5) 0.0431(16) Uani 1 1 d . . . . .
H33 H 0.109578 -0.020828 0.230947 0.052 Uiso 1 1 calc R U . . .
C34 C -0.0497(7) 0.1986(5) 0.3195(7) 0.060(2) Uani 1 1 d . . . . .
H34A H -0.122452 0.193661 0.289350 0.090 Uiso 1 1 calc R U . . .
H34B H -0.026615 0.238804 0.311112 0.090 Uiso 1 1 calc R U . . .
H34C H -0.046262 0.190396 0.384394 0.090 Uiso 1 1 calc R U . . .
C35 C 0.2599(5) 0.1466(3) 0.4352(4) 0.0328(13) Uani 1 1 d . . . . .
H35A H 0.272661 0.181927 0.473767 0.039 Uiso 1 1 calc R U . . .
H35B H 0.183026 0.138995 0.427056 0.039 Uiso 1 1 calc R U . . .
C36 C 0.2651(7) 0.0124(4) 0.4626(6) 0.0511(19) Uani 1 1 d . . . . .
H36A H 0.188460 0.014752 0.460995 0.077 Uiso 1 1 calc R U . . .
H36B H 0.293730 -0.018133 0.505409 0.077 Uiso 1 1 calc R U . . .
H36C H 0.281129 0.002876 0.401959 0.077 Uiso 1 1 calc R U . . .
C37 C 0.3127(7) 0.0924(4) 0.6232(5) 0.051(2) Uani 1 1 d . . . . .
H37A H 0.352143 0.126914 0.648079 0.077 Uiso 1 1 calc R U . . .
H37B H 0.340850 0.057481 0.656290 0.077 Uiso 1 1 calc R U . . .
H37C H 0.238016 0.097074 0.629367 0.077 Uiso 1 1 calc R U . . .
C38 C 0.4709(6) 0.0829(5) 0.4973(7) 0.057(2) Uani 1 1 d . . . . .
H38A H 0.484275 0.079608 0.434393 0.085 Uiso 1 1 calc R U . . .
H38B H 0.502079 0.049297 0.532227 0.085 Uiso 1 1 calc R U . . .
H38C H 0.502736 0.119082 0.523985 0.085 Uiso 1 1 calc R U . . .
C39 C 0.3945(5) 0.2345(3) 0.3737(4) 0.0324(13) Uani 1 1 d . . . . .
H39A H 0.451363 0.215820 0.416243 0.039 Uiso 1 1 calc R U . . .
H39B H 0.428748 0.253609 0.325980 0.039 Uiso 1 1 calc R U . . .
C40 C 0.1924(6) 0.3008(4) 0.4083(7) 0.054(2) Uani 1 1 d . . . . .
H40A H 0.173323 0.305394 0.342543 0.081 Uiso 1 1 calc R U . . .
H40B H 0.169301 0.335390 0.439003 0.081 Uiso 1 1 calc R U . . .
H40C H 0.157856 0.265942 0.428328 0.081 Uiso 1 1 calc R U . . .
C41 C 0.3706(7) 0.2800(5) 0.5620(5) 0.057(2) Uani 1 1 d . . . . .
H41A H 0.329733 0.246699 0.579306 0.085 Uiso 1 1 calc R U . . .
H41B H 0.353137 0.314997 0.594761 0.085 Uiso 1 1 calc R U . . .
H41C H 0.446144 0.271605 0.577325 0.085 Uiso 1 1 calc R U . . .
C42 C 0.3985(8) 0.3662(4) 0.4177(7) 0.056(2) Uani 1 1 d . . . . .
H42A H 0.450232 0.361692 0.375843 0.085 Uiso 1 1 calc R U . . .
H42B H 0.433636 0.381585 0.475747 0.085 Uiso 1 1 calc R U . . .
H42C H 0.343112 0.393455 0.391770 0.085 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C35 2.046(6) . ?
Pd1 C39 2.103(6) . ?
Pd1 N1 2.235(5) . ?
Pd1 P1 2.3017(17) . ?
P1 C21 1.822(6) . ?
P1 C28 1.831(7) . ?
P1 C2 1.845(7) . ?
Si1 C35 1.853(7) . ?
Si1 C38 1.860(8) . ?
Si1 C36 1.871(8) . ?
Si1 C37 1.881(8) . ?
Si2 C39 1.842(7) . ?
Si2 C40 1.857(8) . ?
Si2 C41 1.878(8) . ?
Si2 C42 1.886(9) . ?
O1 C22 1.362(9) . ?
O1 C27 1.422(10) . ?
O2 C29 1.351(9) . ?
O2 C34 1.428(9) . ?
N1 C1 1.301(8) . ?
N1 C9 1.444(7) . ?
C1 C3 1.476(8) . ?
C1 C2 1.505(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.387(9) . ?
C3 C8 1.400(9) . ?
C4 C5 1.400(10) . ?
C4 H4 0.9500 . ?
C5 C6 1.374(12) . ?
C5 H5 0.9500 . ?
C6 C7 1.363(12) . ?
C6 H6 0.9500 . ?
C7 C8 1.373(9) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C14 1.406(9) . ?
C9 C10 1.405(9) . ?
C10 C11 1.387(9) . ?
C10 C15 1.517(11) . ?
C11 C12 1.372(12) . ?
C11 H11 0.9500 . ?
C12 C13 1.381(12) . ?
C12 H12 0.9500 . ?
C13 C14 1.392(9) . ?
C13 H13 0.9500 . ?
C14 C18 1.521(10) . ?
C15 C16 1.537(11) . ?
C15 C17 1.538(11) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.519(12) . ?
C18 C20 1.536(10) . ?
C18 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C26 1.391(10) . ?
C21 C22 1.414(9) . ?
C22 C23 1.386(10) . ?
C23 C24 1.379(13) . ?
C23 H23 0.9500 . ?
C24 C25 1.391(13) . ?
C24 H24 0.9500 . ?
C25 C26 1.370(11) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.388(10) . ?
C28 C33 1.392(11) . ?
C29 C30 1.392(10) . ?
C30 C31 1.369(15) . ?
C30 H30 0.9500 . ?
C31 C32 1.358(15) . ?
C31 H31 0.9500 . ?
C32 C33 1.391(11) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?

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
C35 Pd1 C39 88.0(3) . . ?
C35 Pd1 N1 174.0(2) . . ?
C39 Pd1 N1 95.7(2) . . ?
C35 Pd1 P1 97.7(2) . . ?
C39 Pd1 P1 174.02(19) . . ?
N1 Pd1 P1 78.50(14) . . ?
C21 P1 C28 105.7(3) . . ?
C21 P1 C2 104.9(3) . . ?
C28 P1 C2 104.5(3) . . ?
C21 P1 Pd1 114.7(2) . . ?
C28 P1 Pd1 128.1(2) . . ?
C2 P1 Pd1 95.6(2) . . ?
C35 Si1 C38 112.7(4) . . ?
C35 Si1 C36 112.4(4) . . ?
C38 Si1 C36 110.7(4) . . ?
C35 Si1 C37 109.4(4) . . ?
C38 Si1 C37 104.8(4) . . ?
C36 Si1 C37 106.3(4) . . ?
C39 Si2 C40 114.3(4) . . ?
C39 Si2 C41 110.2(4) . . ?
C40 Si2 C41 108.3(4) . . ?
C39 Si2 C42 111.5(4) . . ?
C40 Si2 C42 107.5(4) . . ?
C41 Si2 C42 104.5(4) . . ?
C22 O1 C27 117.7(7) . . ?
C29 O2 C34 119.8(6) . . ?
C1 N1 C9 118.3(5) . . ?
C1 N1 Pd1 117.1(4) . . ?
C9 N1 Pd1 124.5(4) . . ?
N1 C1 C3 126.6(6) . . ?
N1 C1 C2 117.3(5) . . ?
C3 C1 C2 116.1(5) . . ?
C1 C2 P1 106.2(4) . . ?
C1 C2 H2A 110.5 . . ?
P1 C2 H2A 110.5 . . ?
C1 C2 H2B 110.5 . . ?
P1 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
C4 C3 C8 117.8(6) . . ?
C4 C3 C1 121.7(6) . . ?
C8 C3 C1 120.4(6) . . ?
C3 C4 C5 120.4(7) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C6 C5 C4 119.8(7) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C7 C6 C5 120.6(7) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C6 C7 C8 120.0(7) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C3 121.5(6) . . ?
C7 C8 H8 119.3 . . ?
C3 C8 H8 119.3 . . ?
C14 C9 C10 121.9(6) . . ?
C14 C9 N1 118.9(5) . . ?
C10 C9 N1 119.1(6) . . ?
C11 C10 C9 117.5(7) . . ?
C11 C10 C15 120.7(6) . . ?
C9 C10 C15 121.8(6) . . ?
C12 C11 C10 121.8(7) . . ?
C12 C11 H11 119.1 . . ?
C10 C11 H11 119.1 . . ?
C11 C12 C13 119.9(7) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C12 C13 C14 121.4(8) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C13 C14 C9 117.4(7) . . ?
C13 C14 C18 118.3(7) . . ?
C9 C14 C18 124.3(6) . . ?
C10 C15 C16 111.9(7) . . ?
C10 C15 C17 111.0(7) . . ?
C16 C15 C17 108.8(7) . . ?
C10 C15 H15 108.3 . . ?
C16 C15 H15 108.3 . . ?
C17 C15 H15 108.3 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C14 111.1(7) . . ?
C19 C18 C20 109.1(7) . . ?
C14 C18 C20 112.0(6) . . ?
C19 C18 H18 108.2 . . ?
C14 C18 H18 108.2 . . ?
C20 C18 H18 108.2 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 C21 C22 117.7(6) . . ?
C26 C21 P1 116.4(5) . . ?
C22 C21 P1 125.6(5) . . ?
O1 C22 C23 123.6(7) . . ?
O1 C22 C21 116.2(6) . . ?
C23 C22 C21 120.2(7) . . ?
C24 C23 C22 120.4(7) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C25 119.8(8) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C26 C25 C24 119.9(8) . . ?
C26 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
C25 C26 C21 121.8(7) . . ?
C25 C26 H26 119.1 . . ?
C21 C26 H26 119.1 . . ?
O1 C27 H27A 109.5 . . ?
O1 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
O1 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C33 120.1(7) . . ?
C29 C28 P1 117.8(6) . . ?
C33 C28 P1 122.0(6) . . ?
O2 C29 C28 116.8(6) . . ?
O2 C29 C30 124.3(7) . . ?
C28 C29 C30 118.9(8) . . ?
C31 C30 C29 119.9(9) . . ?
C31 C30 H30 120.0 . . ?
C29 C30 H30 120.0 . . ?
C32 C31 C30 122.0(8) . . ?
C32 C31 H31 119.0 . . ?
C30 C31 H31 119.0 . . ?
C31 C32 C33 119.1(9) . . ?
C31 C32 H32 120.5 . . ?
C33 C32 H32 120.5 . . ?
C28 C33 C32 120.0(8) . . ?
C28 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
O2 C34 H34A 109.5 . . ?
O2 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
O2 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
Si1 C35 Pd1 119.3(3) . . ?
Si1 C35 H35A 107.5 . . ?
Pd1 C35 H35A 107.5 . . ?
Si1 C35 H35B 107.5 . . ?
Pd1 C35 H35B 107.5 . . ?
H35A C35 H35B 107.0 . . ?
Si1 C36 H36A 109.5 . . ?
Si1 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
Si1 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
Si1 C37 H37A 109.5 . . ?
Si1 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
Si1 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
Si1 C38 H38A 109.5 . . ?
Si1 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
Si1 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
Si2 C39 Pd1 121.0(3) . . ?
Si2 C39 H39A 107.1 . . ?
Pd1 C39 H39A 107.1 . . ?
Si2 C39 H39B 107.1 . . ?
Pd1 C39 H39B 107.1 . . ?
H39A C39 H39B 106.8 . . ?
Si2 C40 H40A 109.5 . . ?
Si2 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
Si2 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
Si2 C41 H41A 109.5 . . ?
Si2 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
Si2 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
Si2 C42 H42A 109.5 . . ?
Si2 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
Si2 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?

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
C9 N1 C1 C3 9.3(9) . . . . ?
Pd1 N1 C1 C3 -173.8(5) . . . . ?
C9 N1 C1 C2 -169.8(5) . . . . ?
Pd1 N1 C1 C2 7.2(7) . . . . ?
N1 C1 C2 P1 -41.3(7) . . . . ?
C3 C1 C2 P1 139.5(5) . . . . ?
C21 P1 C2 C1 -66.7(5) . . . . ?
C28 P1 C2 C1 -177.6(4) . . . . ?
Pd1 P1 C2 C1 50.8(4) . . . . ?
N1 C1 C3 C4 46.5(10) . . . . ?
C2 C1 C3 C4 -134.5(7) . . . . ?
N1 C1 C3 C8 -136.8(7) . . . . ?
C2 C1 C3 C8 42.3(9) . . . . ?
C8 C3 C4 C5 -0.1(12) . . . . ?
C1 C3 C4 C5 176.7(7) . . . . ?
C3 C4 C5 C6 0.6(14) . . . . ?
C4 C5 C6 C7 -0.4(15) . . . . ?
C5 C6 C7 C8 -0.2(14) . . . . ?
C6 C7 C8 C3 0.7(13) . . . . ?
C4 C3 C8 C7 -0.5(11) . . . . ?
C1 C3 C8 C7 -177.4(7) . . . . ?
C1 N1 C9 C14 70.1(7) . . . . ?
Pd1 N1 C9 C14 -106.6(6) . . . . ?
C1 N1 C9 C10 -112.4(7) . . . . ?
Pd1 N1 C9 C10 70.9(6) . . . . ?
C14 C9 C10 C11 -2.0(9) . . . . ?
N1 C9 C10 C11 -179.4(5) . . . . ?
C14 C9 C10 C15 178.9(6) . . . . ?
N1 C9 C10 C15 1.5(9) . . . . ?
C9 C10 C11 C12 1.6(10) . . . . ?
C15 C10 C11 C12 -179.4(7) . . . . ?
C10 C11 C12 C13 0.0(11) . . . . ?
C11 C12 C13 C14 -1.3(11) . . . . ?
C12 C13 C14 C9 0.8(10) . . . . ?
C12 C13 C14 C18 -179.0(7) . . . . ?
C10 C9 C14 C13 0.9(9) . . . . ?
N1 C9 C14 C13 178.3(6) . . . . ?
C10 C9 C14 C18 -179.4(6) . . . . ?
N1 C9 C14 C18 -1.9(9) . . . . ?
C11 C10 C15 C16 -52.6(9) . . . . ?
C9 C10 C15 C16 126.5(7) . . . . ?
C11 C10 C15 C17 69.2(8) . . . . ?
C9 C10 C15 C17 -111.8(7) . . . . ?
C13 C14 C18 C19 -70.5(9) . . . . ?
C9 C14 C18 C19 109.7(8) . . . . ?
C13 C14 C18 C20 51.8(9) . . . . ?
C9 C14 C18 C20 -128.0(7) . . . . ?
C28 P1 C21 C26 -112.5(6) . . . . ?
C2 P1 C21 C26 137.5(6) . . . . ?
Pd1 P1 C21 C26 34.0(6) . . . . ?
C28 P1 C21 C22 74.0(7) . . . . ?
C2 P1 C21 C22 -36.0(7) . . . . ?
Pd1 P1 C21 C22 -139.5(6) . . . . ?
C27 O1 C22 C23 -14.8(13) . . . . ?
C27 O1 C22 C21 165.5(8) . . . . ?
C26 C21 C22 O1 176.2(7) . . . . ?
P1 C21 C22 O1 -10.4(10) . . . . ?
C26 C21 C22 C23 -3.5(11) . . . . ?
P1 C21 C22 C23 169.9(7) . . . . ?
O1 C22 C23 C24 -175.9(9) . . . . ?
C21 C22 C23 C24 3.8(14) . . . . ?
C22 C23 C24 C25 0.2(15) . . . . ?
C23 C24 C25 C26 -4.6(16) . . . . ?
C24 C25 C26 C21 4.9(15) . . . . ?
C22 C21 C26 C25 -0.9(12) . . . . ?
P1 C21 C26 C25 -174.9(7) . . . . ?
C21 P1 C28 C29 -174.3(5) . . . . ?
C2 P1 C28 C29 -64.0(6) . . . . ?
Pd1 P1 C28 C29 45.3(6) . . . . ?
C21 P1 C28 C33 10.1(6) . . . . ?
C2 P1 C28 C33 120.5(6) . . . . ?
Pd1 P1 C28 C33 -130.3(5) . . . . ?
C34 O2 C29 C28 -172.2(7) . . . . ?
C34 O2 C29 C30 6.9(12) . . . . ?
C33 C28 C29 O2 -179.4(6) . . . . ?
P1 C28 C29 O2 5.0(9) . . . . ?
C33 C28 C29 C30 1.4(11) . . . . ?
P1 C28 C29 C30 -174.2(6) . . . . ?
O2 C29 C30 C31 179.8(9) . . . . ?
C28 C29 C30 C31 -1.1(13) . . . . ?
C29 C30 C31 C32 0.7(17) . . . . ?
C30 C31 C32 C33 -0.7(16) . . . . ?
C29 C28 C33 C32 -1.4(11) . . . . ?
P1 C28 C33 C32 174.1(6) . . . . ?
C31 C32 C33 C28 1.0(13) . . . . ?
C38 Si1 C35 Pd1 43.8(6) . . . . ?
C36 Si1 C35 Pd1 -82.3(5) . . . . ?
C37 Si1 C35 Pd1 159.9(4) . . . . ?
C40 Si2 C39 Pd1 -19.1(6) . . . . ?
C41 Si2 C39 Pd1 103.1(5) . . . . ?
C42 Si2 C39 Pd1 -141.3(4) . . . . ?

_refine_diff_density_max         3.127
_refine_diff_density_min         -3.406
_refine_diff_density_rms         0.181


