# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_1Si
_database_code_depnum_ccdc_archive 'CCDC 2001500'
loop_
_audit_author_name
_audit_author_address
'Javier A. Cabeza'
;Universidad de Oviedo
Spain
;
_audit_update_record             
;
2020-05-06 deposited with the CCDC.	2020-06-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H46 N3 P Si'
_chemical_formula_sum            'C28 H46 N3 P Si'
_chemical_formula_weight         483.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   8.833(5)
_cell_length_b                   18.065(5)
_cell_length_c                   18.265(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.564(5)
_cell_angle_gamma                90
_cell_volume                     2905(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9767
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      28.28

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_F_000             1056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.093
_exptl_absorpt_coefficient_mu    0.156
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7085
_exptl_absorpt_correction_T_max  0.7371
_exptl_absorpt_process_details   
; 
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction 

Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Incoatec high brillance I\muS microsource'
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            59980
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.237
_diffrn_reflns_theta_max         28.350
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7251
_reflns_number_gt                6123
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'BRUKER APEX3'
_computing_cell_refinement       'BRUKER APEX3'
_computing_data_reduction        'BRUKER APEX3'
_computing_structure_solution    'SIR-97 (Giacovazzo, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    
'MERCURY (Cambridge Crystallographic Data Centre: Cambridge, UK, 2019)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'

_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)+(0.0492P)²+1.1423P] 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         7251
_refine_ls_number_parameters     310
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0384
_refine_ls_wR_factor_ref         0.0985
_refine_ls_wR_factor_gt          0.0930
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.24498(16) 0.25383(8) 0.16359(7) 0.0210(3) Uani 1 1 d . . . . .
H1A H 0.2879 0.2054 0.1592 0.032 Uiso 1 1 calc R U . . .
H1B H 0.1573 0.2508 0.1913 0.032 Uiso 1 1 calc R U . . .
H1C H 0.3189 0.2860 0.1884 0.032 Uiso 1 1 calc R U . . .
C2 C 0.08317(17) 0.23241(9) 0.04740(8) 0.0275(3) Uani 1 1 d . . . . .
H2A H 0.0595 0.2495 -0.0020 0.041 Uiso 1 1 calc R U . . .
H2B H -0.0077 0.2315 0.0729 0.041 Uiso 1 1 calc R U . . .
H2C H 0.1252 0.1835 0.0463 0.041 Uiso 1 1 calc R U . . .
C3 C 0.13005(17) 0.36129(8) 0.09485(8) 0.0250(3) Uani 1 1 d . . . . .
H3A H 0.2065 0.3944 0.1160 0.038 Uiso 1 1 calc R U . . .
H3B H 0.0479 0.3585 0.1261 0.038 Uiso 1 1 calc R U . . .
H3C H 0.0926 0.3793 0.0473 0.038 Uiso 1 1 calc R U . . .
C4 C 0.19852(14) 0.28460(7) 0.08702(7) 0.0145(2) Uani 1 1 d . . . . .
C5 C 0.37197(14) 0.32043(7) -0.01359(6) 0.0127(2) Uani 1 1 d . . . . .
C6 C 0.27577(14) 0.37596(7) -0.05613(7) 0.0140(2) Uani 1 1 d . . . . .
C7 C 0.16521(15) 0.35332(7) -0.11001(7) 0.0178(3) Uani 1 1 d . . . . .
H7 H 0.1519 0.3032 -0.1204 0.021 Uiso 1 1 calc R U . . .
C8 C 0.07469(17) 0.40568(8) -0.14834(8) 0.0249(3) Uani 1 1 d . . . . .
H8 H 0.0006 0.3906 -0.1843 0.030 Uiso 1 1 calc R U . . .
C9 C 0.09476(18) 0.48021(8) -0.13309(8) 0.0267(3) Uani 1 1 d . . . . .
H9 H 0.0342 0.5151 -0.1589 0.032 Uiso 1 1 calc R U . . .
C10 C 0.20474(19) 0.50325(8) -0.07949(8) 0.0261(3) Uani 1 1 d . . . . .
H10 H 0.2181 0.5534 -0.0695 0.031 Uiso 1 1 calc R U . . .
C11 C 0.29480(16) 0.45121(7) -0.04086(8) 0.0202(3) Uani 1 1 d . . . . .
H11 H 0.3681 0.4665 -0.0047 0.024 Uiso 1 1 calc R U . . .
C12 C 0.58817(15) 0.30171(7) -0.09741(7) 0.0167(3) Uani 1 1 d . . . . .
C13 C 0.49747(16) 0.27226(8) -0.16612(7) 0.0200(3) Uani 1 1 d . . . . .
H13A H 0.4686 0.2218 -0.1581 0.030 Uiso 1 1 calc R U . . .
H13B H 0.5589 0.2746 -0.2071 0.030 Uiso 1 1 calc R U . . .
H13C H 0.4080 0.3019 -0.1762 0.030 Uiso 1 1 calc R U . . .
C14 C 0.63016(18) 0.38292(8) -0.10709(8) 0.0258(3) Uani 1 1 d . . . . .
H14A H 0.5393 0.4117 -0.1164 0.039 Uiso 1 1 calc R U . . .
H14B H 0.6919 0.3876 -0.1478 0.039 Uiso 1 1 calc R U . . .
H14C H 0.6857 0.4005 -0.0632 0.039 Uiso 1 1 calc R U . . .
C15 C 0.73337(18) 0.25612(11) -0.08304(9) 0.0355(4) Uani 1 1 d . . . . .
H15A H 0.7891 0.2736 -0.0391 0.053 Uiso 1 1 calc R U . . .
H15B H 0.7948 0.2612 -0.1238 0.053 Uiso 1 1 calc R U . . .
H15C H 0.7075 0.2050 -0.0771 0.053 Uiso 1 1 calc R U . . .
C16 C 0.65053(15) 0.30267(7) 0.14130(7) 0.0157(3) Uani 1 1 d . . . . .
H16 H 0.5976 0.3460 0.1289 0.019 Uiso 1 1 calc R U . . .
C17 C 0.76254(15) 0.29600(7) 0.19695(7) 0.0161(3) Uani 1 1 d . . . . .
H17 H 0.7990 0.3333 0.2287 0.019 Uiso 1 1 calc R U . . .
C18 C 0.81282(15) 0.22107(7) 0.19702(7) 0.0148(2) Uani 1 1 d . . . . .
H18 H 0.8882 0.2004 0.2291 0.018 Uiso 1 1 calc R U . . .
C19 C 0.72998(13) 0.18484(7) 0.14114(6) 0.0119(2) Uani 1 1 d . . . . .
C20 C 0.74862(14) 0.10774(7) 0.11195(6) 0.0132(2) Uani 1 1 d . . . . .
H20A H 0.8393 0.1065 0.0853 0.016 Uiso 1 1 calc R U . . .
H20B H 0.6627 0.0968 0.0772 0.016 Uiso 1 1 calc R U . . .
C21 C 0.88170(14) -0.03630(7) 0.13507(7) 0.0161(3) Uani 1 1 d . . . . .
C22 C 0.84529(16) -0.04662(8) 0.05216(7) 0.0205(3) Uani 1 1 d . . . . .
H22A H 0.9216 -0.0772 0.0329 0.031 Uiso 1 1 calc R U . . .
H22B H 0.8436 0.0008 0.0283 0.031 Uiso 1 1 calc R U . . .
H22C H 0.7478 -0.0699 0.0434 0.031 Uiso 1 1 calc R U . . .
C23 C 1.04561(15) -0.00690(8) 0.14815(8) 0.0223(3) Uani 1 1 d . . . . .
H23A H 1.1141 -0.0406 0.1271 0.034 Uiso 1 1 calc R U . . .
H23B H 1.0722 -0.0026 0.2000 0.034 Uiso 1 1 calc R U . . .
H23C H 1.0525 0.0408 0.1255 0.034 Uiso 1 1 calc R U . . .
C24 C 0.87557(17) -0.11188(8) 0.17324(8) 0.0249(3) Uani 1 1 d . . . . .
H24A H 0.7777 -0.1340 0.1617 0.037 Uiso 1 1 calc R U . . .
H24B H 0.8922 -0.1054 0.2254 0.037 Uiso 1 1 calc R U . . .
H24C H 0.9529 -0.1436 0.1565 0.037 Uiso 1 1 calc R U . . .
C25 C 0.56044(14) -0.00036(7) 0.18175(7) 0.0140(2) Uani 1 1 d . . . . .
C26 C 0.46435(15) 0.06868(7) 0.19416(7) 0.0180(3) Uani 1 1 d . . . . .
H26A H 0.4570 0.0984 0.1505 0.027 Uiso 1 1 calc R U . . .
H26B H 0.5114 0.0969 0.2343 0.027 Uiso 1 1 calc R U . . .
H26C H 0.3645 0.0539 0.2055 0.027 Uiso 1 1 calc R U . . .
C27 C 0.49553(15) -0.03862(8) 0.11143(8) 0.0200(3) Uani 1 1 d . . . . .
H27A H 0.3897 -0.0489 0.1150 0.030 Uiso 1 1 calc R U . . .
H27B H 0.5491 -0.0841 0.1051 0.030 Uiso 1 1 calc R U . . .
H27C H 0.5070 -0.0068 0.0701 0.030 Uiso 1 1 calc R U . . .
C28 C 0.54830(17) -0.05219(8) 0.24771(8) 0.0222(3) Uani 1 1 d . . . . .
H28A H 0.4438 -0.0652 0.2515 0.033 Uiso 1 1 calc R U . . .
H28B H 0.5870 -0.0275 0.2919 0.033 Uiso 1 1 calc R U . . .
H28C H 0.6065 -0.0962 0.2410 0.033 Uiso 1 1 calc R U . . .
N1 N 0.33975(12) 0.28586(6) 0.04828(6) 0.0129(2) Uani 1 1 d . . . . .
N2 N 0.50364(12) 0.29160(6) -0.03133(6) 0.0150(2) Uani 1 1 d . . . . .
N3 N 0.62782(12) 0.23491(6) 0.10610(6) 0.0130(2) Uani 1 1 d . . . . .
P1 P 0.76348(4) 0.03335(2) 0.18318(2) 0.01149(8) Uani 1 1 d . . . . .
Si1 Si 0.48415(4) 0.21261(2) 0.03333(2) 0.01281(9) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C4 1.5304(18) . ?
C2 C4 1.5275(19) . ?
C3 C4 1.5231(19) . ?
C4 N1 1.4825(17) . ?
C5 N2 1.3374(17) . ?
C5 N1 1.3413(16) . ?
C5 C6 1.4924(17) . ?
C5 Si1 2.3183(14) . ?
C6 C7 1.3917(18) . ?
C6 C11 1.3951(18) . ?
C7 C8 1.3911(19) . ?
C8 C9 1.383(2) . ?
C9 C10 1.387(2) . ?
C10 C11 1.387(2) . ?
C12 N2 1.4802(16) . ?
C12 C14 1.527(2) . ?
C12 C15 1.529(2) . ?
C12 C13 1.5297(18) . ?
C16 C17 1.3662(19) . ?
C16 N3 1.3898(16) . ?
C17 C18 1.4246(18) . ?
C18 C19 1.3735(17) . ?
C19 N3 1.3965(16) . ?
C19 C20 1.5051(17) . ?
C20 P1 1.8678(13) . ?
C21 C22 1.5342(19) . ?
C21 C24 1.5360(19) . ?
C21 C23 1.543(2) . ?
C21 P1 1.8952(14) . ?
C25 C27 1.5293(18) . ?
C25 C26 1.5355(18) . ?
C25 C28 1.5363(18) . ?
C25 P1 1.8923(16) . ?
N1 Si1 1.8729(12) . ?
N2 Si1 1.8690(12) . ?
N3 Si1 1.8085(12) . ?

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
N1 C4 C3 112.73(11) . . ?
N1 C4 C2 109.77(10) . . ?
C3 C4 C2 110.55(12) . . ?
N1 C4 C1 105.49(10) . . ?
C3 C4 C1 108.92(11) . . ?
C2 C4 C1 109.21(11) . . ?
N2 C5 N1 105.65(10) . . ?
N2 C5 C6 127.28(11) . . ?
N1 C5 C6 126.97(11) . . ?
N2 C5 Si1 53.71(6) . . ?
N1 C5 Si1 53.88(6) . . ?
C6 C5 Si1 165.05(9) . . ?
C7 C6 C11 119.63(12) . . ?
C7 C6 C5 120.60(11) . . ?
C11 C6 C5 119.76(11) . . ?
C8 C7 C6 119.93(13) . . ?
C9 C8 C7 120.07(13) . . ?
C8 C9 C10 120.36(13) . . ?
C9 C10 C11 119.78(13) . . ?
C10 C11 C6 120.23(13) . . ?
N2 C12 C14 110.85(11) . . ?
N2 C12 C15 105.32(11) . . ?
C14 C12 C15 109.22(13) . . ?
N2 C12 C13 111.15(11) . . ?
C14 C12 C13 110.81(11) . . ?
C15 C12 C13 109.32(12) . . ?
C17 C16 N3 109.62(11) . . ?
C16 C17 C18 106.96(11) . . ?
C19 C18 C17 107.72(11) . . ?
C18 C19 N3 108.58(11) . . ?
C18 C19 C20 129.59(11) . . ?
N3 C19 C20 121.46(11) . . ?
C19 C20 P1 115.01(8) . . ?
C22 C21 C24 109.14(11) . . ?
C22 C21 C23 108.37(11) . . ?
C24 C21 C23 107.59(11) . . ?
C22 C21 P1 117.28(9) . . ?
C24 C21 P1 109.82(9) . . ?
C23 C21 P1 104.15(9) . . ?
C27 C25 C26 108.44(11) . . ?
C27 C25 C28 109.77(11) . . ?
C26 C25 C28 107.79(10) . . ?
C27 C25 P1 116.66(9) . . ?
C26 C25 P1 105.72(9) . . ?
C28 C25 P1 108.09(9) . . ?
C5 N1 C4 130.71(11) . . ?
C5 N1 Si1 90.77(8) . . ?
C4 N1 Si1 131.87(8) . . ?
C5 N2 C12 130.87(11) . . ?
C5 N2 Si1 91.06(8) . . ?
C12 N2 Si1 133.41(9) . . ?
C16 N3 C19 107.11(10) . . ?
C16 N3 Si1 127.10(9) . . ?
C19 N3 Si1 125.63(9) . . ?
C20 P1 C25 102.00(6) . . ?
C20 P1 C21 99.53(6) . . ?
C25 P1 C21 109.66(6) . . ?
N3 Si1 N2 101.52(5) . . ?
N3 Si1 N1 100.47(6) . . ?
N2 Si1 N1 69.56(5) . . ?
N3 Si1 C5 109.80(5) . . ?
N2 Si1 C5 35.23(5) . . ?
N1 Si1 C5 35.35(4) . . ?

_refine_diff_density_max         0.346
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.049

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_2Pd-Si
_database_code_depnum_ccdc_archive 'CCDC 2001501'
loop_
_audit_author_name
_audit_author_address
'Javier A. Cabeza'
;Universidad de Oviedo
Spain
;
_audit_update_record             
;
2020-05-06 deposited with the CCDC.	2020-06-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H46 Cl2 N3 P Pd Si, C4 H8 O'
_chemical_formula_sum            'C32 H54 Cl2 N3 O P Pd Si'
_chemical_formula_weight         733.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   18.2783(4)
_cell_length_b                   10.5426(2)
_cell_length_c                   18.3984(4)
_cell_angle_alpha                90
_cell_angle_beta                 94.109(2)
_cell_angle_gamma                90
_cell_volume                     3536.27(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    10159
_cell_measurement_theta_min      4.8530
_cell_measurement_theta_max      69.4580

_exptl_crystal_description       fragment
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_F_000             1536
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    6.591
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.35808
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Nova (Cu) X-ray Source'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15937
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         4.819
_diffrn_reflns_theta_max         69.604
_diffrn_reflns_theta_full        67.680
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6536
_reflns_number_gt                6069
_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       
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_cell_refinement       
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction        
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_structure_solution    'SIR-97 (Giacovazzo, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    
'MERCURY (Cambridge Crystallographic Data Centre: Cambridge, UK, 2018)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'

_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)+(0.0505P)²+9.1132P] 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         6536
_refine_ls_number_parameters     382
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0432
_refine_ls_wR_factor_ref         0.1209
_refine_ls_wR_factor_gt          0.1187
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.9164(3) -0.1522(5) 0.5826(2) 0.0482(11) Uani 1 1 d . . . . .
H1A H 0.9275 -0.0665 0.5661 0.072 Uiso 1 1 calc R U . . .
H1B H 0.9509 -0.1753 0.6238 0.072 Uiso 1 1 calc R U . . .
H1C H 0.8662 -0.1546 0.5981 0.072 Uiso 1 1 calc R U . . .
C2 C 1.0014(3) -0.2426(6) 0.4971(3) 0.0543(13) Uani 1 1 d . . . . .
H2A H 1.0077 -0.3096 0.4611 0.081 Uiso 1 1 calc R U . . .
H2B H 1.0360 -0.2562 0.5396 0.081 Uiso 1 1 calc R U . . .
H2C H 1.0109 -0.1598 0.4753 0.081 Uiso 1 1 calc R U . . .
C3 C 0.9027(4) -0.3776(5) 0.5447(3) 0.0629(15) Uani 1 1 d . . . . .
H3A H 0.8516 -0.3774 0.5575 0.094 Uiso 1 1 calc R U . . .
H3B H 0.9347 -0.4026 0.5873 0.094 Uiso 1 1 calc R U . . .
H3C H 0.9084 -0.4379 0.5049 0.094 Uiso 1 1 calc R U . . .
C4 C 0.9236(2) -0.2458(4) 0.5205(2) 0.0326(8) Uani 1 1 d . . . . .
C5 C 0.8540(2) -0.2487(4) 0.39399(19) 0.0272(8) Uani 1 1 d . . . . .
C6 C 0.8998(2) -0.3376(4) 0.35431(19) 0.0269(7) Uani 1 1 d . . . . .
C7 C 0.9603(2) -0.2920(4) 0.3208(2) 0.0328(8) Uani 1 1 d . . . . .
H7 H 0.9725 -0.2045 0.3234 0.039 Uiso 1 1 calc R U . . .
C8 C 1.0023(2) -0.3745(5) 0.2837(2) 0.0442(11) Uani 1 1 d . . . . .
H8 H 1.0432 -0.3436 0.2598 0.053 Uiso 1 1 calc R U . . .
C9 C 0.9856(3) -0.5011(5) 0.2811(3) 0.0534(13) Uani 1 1 d . . . . .
H9 H 1.0152 -0.5575 0.2555 0.064 Uiso 1 1 calc R U . . .
C10 C 0.9266(3) -0.5475(5) 0.3149(3) 0.0538(13) Uani 1 1 d . . . . .
H10 H 0.9158 -0.6356 0.3132 0.065 Uiso 1 1 calc R U . . .
C11 C 0.8829(2) -0.4657(4) 0.3514(2) 0.0391(9) Uani 1 1 d . . . . .
H11 H 0.8417 -0.4971 0.3744 0.047 Uiso 1 1 calc R U . . .
C12 C 0.7505(2) -0.2005(4) 0.2957(2) 0.0375(9) Uani 1 1 d . . . . .
C13 C 0.8005(3) -0.1666(6) 0.2359(2) 0.0537(13) Uani 1 1 d . . . . .
H13A H 0.8245 -0.0853 0.2474 0.081 Uiso 1 1 calc R U . . .
H13B H 0.7713 -0.1599 0.1893 0.081 Uiso 1 1 calc R U . . .
H13C H 0.8377 -0.2328 0.2327 0.081 Uiso 1 1 calc R U . . .
C14 C 0.7172(3) -0.3307(6) 0.2818(3) 0.0589(14) Uani 1 1 d . . . . .
H14A H 0.7564 -0.3941 0.2816 0.088 Uiso 1 1 calc R U . . .
H14B H 0.6889 -0.3311 0.2345 0.088 Uiso 1 1 calc R U . . .
H14C H 0.6847 -0.3512 0.3203 0.088 Uiso 1 1 calc R U . . .
C15 C 0.6907(3) -0.1008(6) 0.2975(3) 0.0664(18) Uani 1 1 d . . . . .
H15A H 0.6568 -0.1239 0.3343 0.100 Uiso 1 1 calc R U . . .
H15B H 0.6637 -0.0959 0.2495 0.100 Uiso 1 1 calc R U . . .
H15C H 0.7129 -0.0182 0.3097 0.100 Uiso 1 1 calc R U . . .
C16 C 0.6900(2) -0.3059(4) 0.4826(2) 0.0356(9) Uani 1 1 d . . . . .
H16 H 0.7058 -0.3612 0.4461 0.043 Uiso 1 1 calc R U . . .
C17 C 0.6348(2) -0.3300(4) 0.5259(2) 0.0375(9) Uani 1 1 d . . . . .
H17 H 0.6049 -0.4039 0.5247 0.045 Uiso 1 1 calc R U . . .
C18 C 0.6297(2) -0.2247(4) 0.5732(2) 0.0307(8) Uani 1 1 d . . . . .
H18 H 0.5955 -0.2151 0.6093 0.037 Uiso 1 1 calc R U . . .
C19 C 0.6823(2) -0.1399(3) 0.55770(18) 0.0246(7) Uani 1 1 d . . . . .
C20 C 0.7059(2) -0.0223(3) 0.59756(18) 0.0252(7) Uani 1 1 d . . . . .
H20A H 0.7539 -0.0396 0.6242 0.030 Uiso 1 1 calc R U . . .
H20B H 0.6704 -0.0055 0.6345 0.030 Uiso 1 1 calc R U . . .
C21 C 0.6174(2) 0.1714(4) 0.5182(2) 0.0291(8) Uani 1 1 d . . . . .
C22 C 0.5977(2) 0.1118(4) 0.4432(2) 0.0371(9) Uani 1 1 d . . . . .
H22A H 0.6039 0.0196 0.4464 0.056 Uiso 1 1 calc R U . . .
H22B H 0.6299 0.1461 0.4077 0.056 Uiso 1 1 calc R U . . .
H22C H 0.5465 0.1315 0.4276 0.056 Uiso 1 1 calc R U . . .
C23 C 0.5635(2) 0.1228(4) 0.5720(2) 0.0355(9) Uani 1 1 d . . . . .
H23A H 0.5140 0.1528 0.5570 0.053 Uiso 1 1 calc R U . . .
H23B H 0.5781 0.1547 0.6210 0.053 Uiso 1 1 calc R U . . .
H23C H 0.5641 0.0298 0.5725 0.053 Uiso 1 1 calc R U . . .
C24 C 0.6086(3) 0.3154(4) 0.5125(3) 0.0424(10) Uani 1 1 d . . . . .
H24A H 0.6438 0.3493 0.4798 0.064 Uiso 1 1 calc R U . . .
H24B H 0.6177 0.3534 0.5609 0.064 Uiso 1 1 calc R U . . .
H24C H 0.5586 0.3357 0.4932 0.064 Uiso 1 1 calc R U . . .
C25 C 0.7633(2) 0.2288(4) 0.6169(2) 0.0355(9) Uani 1 1 d . . . . .
C26 C 0.7773(4) 0.3621(5) 0.5893(3) 0.0661(16) Uani 1 1 d . . . . .
H26A H 0.7304 0.4050 0.5777 0.099 Uiso 1 1 calc R U . . .
H26B H 0.8046 0.3572 0.5455 0.099 Uiso 1 1 calc R U . . .
H26C H 0.8060 0.4099 0.6271 0.099 Uiso 1 1 calc R U . . .
C27 C 0.7219(3) 0.2353(5) 0.6859(2) 0.0500(12) Uani 1 1 d . . . . .
H27A H 0.7511 0.2827 0.7235 0.075 Uiso 1 1 calc R U . . .
H27B H 0.7132 0.1492 0.7033 0.075 Uiso 1 1 calc R U . . .
H27C H 0.6748 0.2782 0.6751 0.075 Uiso 1 1 calc R U . . .
C28 C 0.8388(3) 0.1682(6) 0.6354(3) 0.0555(13) Uani 1 1 d . . . . .
H28A H 0.8639 0.1563 0.5906 0.083 Uiso 1 1 calc R U . . .
H28B H 0.8324 0.0858 0.6588 0.083 Uiso 1 1 calc R U . . .
H28C H 0.8681 0.2238 0.6687 0.083 Uiso 1 1 calc R U . . .
C29 C 0.5706(5) -0.5847(7) 0.3131(4) 0.088(2) Uani 1 1 d . . . . .
H29A H 0.6195 -0.5847 0.3399 0.105 Uiso 1 1 calc R U . . .
H29B H 0.5533 -0.6734 0.3079 0.105 Uiso 1 1 calc R U . . .
C30 C 0.5194(6) -0.5102(13) 0.3519(5) 0.146(5) Uani 1 1 d . . . . .
H30A H 0.4813 -0.5659 0.3704 0.176 Uiso 1 1 calc R U . . .
H30B H 0.5455 -0.4670 0.3940 0.176 Uiso 1 1 calc R U . . .
C31 C 0.4866(4) -0.4193(8) 0.3030(4) 0.089(2) Uani 1 1 d . . . . .
H31A H 0.5024 -0.3323 0.3170 0.107 Uiso 1 1 calc R U . . .
H31B H 0.4324 -0.4240 0.3016 0.107 Uiso 1 1 calc R U . . .
C32 C 0.5132(4) -0.4549(9) 0.2323(3) 0.087(2) Uani 1 1 d . . . . .
H32A H 0.4747 -0.5026 0.2032 0.105 Uiso 1 1 calc R U . . .
H32B H 0.5250 -0.3777 0.2047 0.105 Uiso 1 1 calc R U . . .
Cl1 Cl 0.87169(6) 0.07482(12) 0.36069(6) 0.0455(3) Uani 1 1 d . . . . .
Cl2 Cl 0.75991(7) 0.31701(11) 0.40532(7) 0.0529(3) Uani 1 1 d . . . . .
N1 N 0.86911(17) -0.2038(3) 0.46143(16) 0.0292(7) Uani 1 1 d . . . . .
N2 N 0.79002(17) -0.1978(3) 0.36958(16) 0.0285(7) Uani 1 1 d . . . . .
N3 N 0.72033(17) -0.1869(3) 0.50002(17) 0.0280(7) Uani 1 1 d . . . . .
O1 O 0.5743(3) -0.5281(6) 0.2442(2) 0.0947(16) Uani 1 1 d . . . . .
P1 P 0.71518(5) 0.12365(9) 0.54448(5) 0.0236(2) Uani 1 1 d . . . . .
Pd1 Pd 0.78440(2) 0.10415(3) 0.44776(2) 0.02696(11) Uani 1 1 d . . . . .
Si1 Si 0.78734(5) -0.10695(9) 0.45337(5) 0.0251(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C4 1.522(6) . ?
C2 C4 1.517(6) . ?
C3 C4 1.516(7) . ?
C4 N1 1.488(5) . ?
C5 N2 1.335(5) . ?
C5 N1 1.338(5) . ?
C5 C6 1.483(5) . ?
C5 Si1 2.259(4) . ?
C6 C11 1.386(6) . ?
C6 C7 1.390(5) . ?
C7 C8 1.373(6) . ?
C8 C9 1.369(7) . ?
C9 C10 1.373(8) . ?
C10 C11 1.381(7) . ?
C12 N2 1.494(5) . ?
C12 C14 1.517(7) . ?
C12 C15 1.518(7) . ?
C12 C13 1.521(6) . ?
C16 C17 1.354(6) . ?
C16 N3 1.399(5) . ?
C17 C18 1.418(6) . ?
C18 C19 1.358(5) . ?
C19 N3 1.400(5) . ?
C19 C20 1.489(5) . ?
C20 P1 1.837(4) . ?
C21 C24 1.529(5) . ?
C21 C23 1.534(5) . ?
C21 C22 1.536(5) . ?
C21 P1 1.885(4) . ?
C25 C26 1.522(6) . ?
C25 C27 1.525(6) . ?
C25 C28 1.536(7) . ?
C25 P1 1.899(4) . ?
C29 O1 1.408(8) . ?
C29 C30 1.448(12) . ?
C30 C31 1.418(11) . ?
C31 C32 1.470(9) . ?
C32 O1 1.363(8) . ?
Cl1 Pd1 2.3608(10) . ?
Cl2 Pd1 2.4075(11) . ?
N1 Si1 1.807(3) . ?
N2 Si1 1.818(3) . ?
N3 Si1 1.760(3) . ?
P1 Pd1 2.2654(9) . ?
Pd1 Si1 2.2284(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C4 C3 108.5(4) . . ?
N1 C4 C2 112.2(3) . . ?
C3 C4 C2 111.4(4) . . ?
N1 C4 C1 105.5(3) . . ?
C3 C4 C1 109.7(4) . . ?
C2 C4 C1 109.4(4) . . ?
N2 C5 N1 106.7(3) . . ?
N2 C5 C6 126.9(3) . . ?
N1 C5 C6 126.4(3) . . ?
N2 C5 Si1 53.61(18) . . ?
N1 C5 Si1 53.14(19) . . ?
C6 C5 Si1 177.7(3) . . ?
C11 C6 C7 120.1(4) . . ?
C11 C6 C5 120.2(3) . . ?
C7 C6 C5 119.7(3) . . ?
C8 C7 C6 119.5(4) . . ?
C9 C8 C7 120.2(4) . . ?
C8 C9 C10 120.8(4) . . ?
C9 C10 C11 119.9(4) . . ?
C10 C11 C6 119.4(4) . . ?
N2 C12 C14 109.5(4) . . ?
N2 C12 C15 105.6(3) . . ?
C14 C12 C15 110.5(4) . . ?
N2 C12 C13 112.1(3) . . ?
C14 C12 C13 110.2(4) . . ?
C15 C12 C13 108.9(4) . . ?
C17 C16 N3 109.5(3) . . ?
C16 C17 C18 107.3(3) . . ?
C19 C18 C17 108.0(3) . . ?
C18 C19 N3 108.9(3) . . ?
C18 C19 C20 129.0(3) . . ?
N3 C19 C20 121.7(3) . . ?
C19 C20 P1 118.1(2) . . ?
C24 C21 C23 107.8(3) . . ?
C24 C21 C22 109.1(3) . . ?
C23 C21 C22 108.8(3) . . ?
C24 C21 P1 112.1(3) . . ?
C23 C21 P1 112.7(3) . . ?
C22 C21 P1 106.2(3) . . ?
C26 C25 C27 109.9(4) . . ?
C26 C25 C28 106.7(4) . . ?
C27 C25 C28 109.0(4) . . ?
C26 C25 P1 112.7(3) . . ?
C27 C25 P1 112.2(3) . . ?
C28 C25 P1 106.1(3) . . ?
O1 C29 C30 106.8(6) . . ?
C31 C30 C29 108.2(6) . . ?
C30 C31 C32 103.8(6) . . ?
O1 C32 C31 108.7(5) . . ?
C5 N1 C4 130.9(3) . . ?
C5 N1 Si1 90.5(2) . . ?
C4 N1 Si1 137.2(2) . . ?
C5 N2 C12 130.8(3) . . ?
C5 N2 Si1 90.1(2) . . ?
C12 N2 Si1 137.8(3) . . ?
C16 N3 C19 106.3(3) . . ?
C16 N3 Si1 126.6(3) . . ?
C19 N3 Si1 126.9(2) . . ?
C32 O1 C29 107.0(5) . . ?
C20 P1 C21 103.79(17) . . ?
C20 P1 C25 99.88(17) . . ?
C21 P1 C25 113.99(18) . . ?
C20 P1 Pd1 114.80(12) . . ?
C21 P1 Pd1 113.27(12) . . ?
C25 P1 Pd1 110.31(13) . . ?
Si1 Pd1 P1 93.86(3) . . ?
Si1 Pd1 Cl1 83.42(4) . . ?
P1 Pd1 Cl1 170.93(4) . . ?
Si1 Pd1 Cl2 161.67(4) . . ?
P1 Pd1 Cl2 93.95(4) . . ?
Cl1 Pd1 Cl2 91.20(4) . . ?
N3 Si1 N1 106.84(15) . . ?
N3 Si1 N2 102.90(15) . . ?
N1 Si1 N2 72.53(14) . . ?
N3 Si1 Pd1 119.05(11) . . ?
N1 Si1 Pd1 125.80(11) . . ?
N2 Si1 Pd1 119.24(11) . . ?
N3 Si1 C5 109.72(14) . . ?
N1 Si1 C5 36.33(13) . . ?
N2 Si1 C5 36.24(14) . . ?
Pd1 Si1 C5 130.57(10) . . ?

_refine_diff_density_max         0.787
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.098

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_4Pd-Si
_database_code_depnum_ccdc_archive 'CCDC 2001503'
loop_
_audit_author_name
_audit_author_address
'Javier A. Cabeza'
;Universidad de Oviedo
Spain
;
_audit_update_record             
;
2020-05-06 deposited with the CCDC.	2020-06-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H61 N3 P2 Pd Si'
_chemical_formula_sum            'C46 H61 N3 P2 Pd Si'
_chemical_formula_weight         852.40

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

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

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

_cell_length_a                   18.1593(2)
_cell_length_b                   20.9946(2)
_cell_length_c                   23.5554(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8980.43(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    17873
_cell_measurement_theta_min      3.7170
_cell_measurement_theta_max      69.4620

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_F_000             3584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    4.510
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.37259
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Nova (Cu) X-ray Source'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26822
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.725
_diffrn_reflns_theta_max         69.526
_diffrn_reflns_theta_full        67.680
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             8279
_reflns_number_gt                7706
_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       
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_cell_refinement       
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction        
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_structure_solution    'SIR-97 (Giacovazzo, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    
'MERCURY (Cambridge Crystallographic Data Centre: Cambridge, UK, 2018)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'

_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)+(0.0393P)²+2.0034P] 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         8279
_refine_ls_number_parameters     490
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0255
_refine_ls_wR_factor_ref         0.0677
_refine_ls_wR_factor_gt          0.0662
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.74292(10) -0.00294(10) 0.25299(8) 0.0429(4) Uani 1 1 d . . . . .
H1A H 0.7268 0.0289 0.2252 0.064 Uiso 1 1 calc R U . . .
H1B H 0.6998 -0.0252 0.2683 0.064 Uiso 1 1 calc R U . . .
H1C H 0.7756 -0.0337 0.2344 0.064 Uiso 1 1 calc R U . . .
C2 C 0.73343(10) 0.07794(10) 0.32998(9) 0.0456(4) Uani 1 1 d . . . . .
H2A H 0.7592 0.0979 0.3619 0.068 Uiso 1 1 calc R U . . .
H2B H 0.6893 0.0560 0.3439 0.068 Uiso 1 1 calc R U . . .
H2C H 0.7190 0.1108 0.3025 0.068 Uiso 1 1 calc R U . . .
C3 C 0.81051(11) -0.01975(10) 0.34381(8) 0.0413(4) Uani 1 1 d . . . . .
H3A H 0.8471 -0.0474 0.3257 0.062 Uiso 1 1 calc R U . . .
H3B H 0.7686 -0.0454 0.3565 0.062 Uiso 1 1 calc R U . . .
H3C H 0.8328 0.0016 0.3766 0.062 Uiso 1 1 calc R U . . .
C4 C 0.78417(9) 0.03003(8) 0.30131(7) 0.0304(3) Uani 1 1 d . . . . .
C5 C 0.90460(8) 0.09394(8) 0.29618(6) 0.0276(3) Uani 1 1 d . . . . .
C6 C 0.91423(9) 0.11327(9) 0.35656(7) 0.0328(4) Uani 1 1 d . . . . .
C7 C 0.88181(12) 0.16872(11) 0.37613(9) 0.0480(5) Uani 1 1 d . . . . .
H7 H 0.8540 0.1947 0.3510 0.058 Uiso 1 1 calc R U . . .
C8 C 0.89002(15) 0.18641(13) 0.43269(11) 0.0677(7) Uani 1 1 d . . . . .
H8 H 0.8678 0.2245 0.4462 0.081 Uiso 1 1 calc R U . . .
C9 C 0.93010(14) 0.14896(15) 0.46896(9) 0.0701(8) Uani 1 1 d . . . . .
H9 H 0.9352 0.1610 0.5076 0.084 Uiso 1 1 calc R U . . .
C10 C 0.96285(11) 0.09431(15) 0.44976(8) 0.0613(7) Uani 1 1 d . . . . .
H10 H 0.9911 0.0689 0.4751 0.074 Uiso 1 1 calc R U . . .
C11 C 0.95496(10) 0.07584(11) 0.39342(7) 0.0436(5) Uani 1 1 d . . . . .
H11 H 0.9774 0.0377 0.3803 0.052 Uiso 1 1 calc R U . . .
C12 C 1.01060(10) 0.15395(9) 0.24840(7) 0.0367(4) Uani 1 1 d . . . . .
C13 C 0.98588(13) 0.22210(10) 0.26034(10) 0.0522(5) Uani 1 1 d . . . . .
H13A H 0.9440 0.2327 0.2359 0.078 Uiso 1 1 calc R U . . .
H13B H 1.0266 0.2515 0.2526 0.078 Uiso 1 1 calc R U . . .
H13C H 0.9711 0.2259 0.3002 0.078 Uiso 1 1 calc R U . . .
C14 C 1.07203(11) 0.13390(12) 0.28857(9) 0.0536(6) Uani 1 1 d . . . . .
H14A H 1.0554 0.1388 0.3279 0.080 Uiso 1 1 calc R U . . .
H14B H 1.1154 0.1608 0.2822 0.080 Uiso 1 1 calc R U . . .
H14C H 1.0849 0.0893 0.2815 0.080 Uiso 1 1 calc R U . . .
C15 C 1.03792(10) 0.14890(10) 0.18706(8) 0.0426(4) Uani 1 1 d . . . . .
H15A H 1.0531 0.1050 0.1792 0.064 Uiso 1 1 calc R U . . .
H15B H 1.0800 0.1775 0.1816 0.064 Uiso 1 1 calc R U . . .
H15C H 0.9982 0.1610 0.1611 0.064 Uiso 1 1 calc R U . . .
C16 C 0.97694(10) -0.02044(9) 0.20028(8) 0.0379(4) Uani 1 1 d . . . . .
H16 H 1.0022 -0.0067 0.2334 0.046 Uiso 1 1 calc R U . . .
C17 C 0.99473(10) -0.07283(9) 0.16906(8) 0.0419(4) Uani 1 1 d . . . . .
H17 H 1.0340 -0.1016 0.1762 0.050 Uiso 1 1 calc R U . . .
C18 C 0.94364(11) -0.07608(9) 0.12400(8) 0.0380(4) Uani 1 1 d . . . . .
H18 H 0.9423 -0.1078 0.0952 0.046 Uiso 1 1 calc R U . . .
C19 C 0.89628(9) -0.02560(8) 0.12899(6) 0.0297(3) Uani 1 1 d . . . . .
C20 C 0.82947(10) -0.01416(8) 0.09301(7) 0.0326(3) Uani 1 1 d . . . . .
H20A H 0.7860 -0.0266 0.1158 0.039 Uiso 1 1 calc R U . . .
H20B H 0.8321 -0.0441 0.0606 0.039 Uiso 1 1 calc R U . . .
C21 C 0.87738(9) 0.07447(9) 0.00263(7) 0.0336(4) Uani 1 1 d . . . . .
C22 C 0.95401(9) 0.07309(10) 0.03053(8) 0.0393(4) Uani 1 1 d . . . . .
H22A H 0.9627 0.0310 0.0471 0.059 Uiso 1 1 calc R U . . .
H22B H 0.9564 0.1055 0.0604 0.059 Uiso 1 1 calc R U . . .
H22C H 0.9917 0.0819 0.0018 0.059 Uiso 1 1 calc R U . . .
C23 C 0.87258(11) 0.02224(11) -0.04258(8) 0.0463(5) Uani 1 1 d . . . . .
H23A H 0.8252 0.0252 -0.0623 0.069 Uiso 1 1 calc R U . . .
H23B H 0.8769 -0.0196 -0.0244 0.069 Uiso 1 1 calc R U . . .
H23C H 0.9127 0.0277 -0.0700 0.069 Uiso 1 1 calc R U . . .
C24 C 0.86903(13) 0.14000(10) -0.02505(9) 0.0510(5) Uani 1 1 d . . . . .
H24A H 0.9120 0.1486 -0.0491 0.077 Uiso 1 1 calc R U . . .
H24B H 0.8655 0.1727 0.0045 0.077 Uiso 1 1 calc R U . . .
H24C H 0.8243 0.1407 -0.0483 0.077 Uiso 1 1 calc R U . . .
C25 C 0.71324(10) 0.05243(10) 0.03659(7) 0.0388(4) Uani 1 1 d . . . . .
C26 C 0.66500(10) 0.05999(12) 0.08994(9) 0.0498(5) Uani 1 1 d . . . . .
H26A H 0.6130 0.0562 0.0794 0.075 Uiso 1 1 calc R U . . .
H26B H 0.6738 0.1019 0.1069 0.075 Uiso 1 1 calc R U . . .
H26C H 0.6775 0.0267 0.1174 0.075 Uiso 1 1 calc R U . . .
C27 C 0.69171(11) 0.10532(12) -0.00518(9) 0.0492(5) Uani 1 1 d . . . . .
H27A H 0.7168 0.0984 -0.0415 0.074 Uiso 1 1 calc R U . . .
H27B H 0.7063 0.1467 0.0104 0.074 Uiso 1 1 calc R U . . .
H27C H 0.6383 0.1046 -0.0111 0.074 Uiso 1 1 calc R U . . .
C28 C 0.69801(12) -0.01256(11) 0.01026(9) 0.0512(5) Uani 1 1 d . . . . .
H28A H 0.6473 -0.0139 -0.0038 0.077 Uiso 1 1 calc R U . . .
H28B H 0.7048 -0.0458 0.0390 0.077 Uiso 1 1 calc R U . . .
H28C H 0.7321 -0.0198 -0.0213 0.077 Uiso 1 1 calc R U . . .
C29 C 0.85573(9) 0.30055(9) 0.13431(7) 0.0328(4) Uani 1 1 d . . . . .
C30 C 0.92193(9) 0.27749(9) 0.11316(7) 0.0367(4) Uani 1 1 d . . . . .
H30 H 0.9242 0.2351 0.0991 0.044 Uiso 1 1 calc R U . . .
C31 C 0.98465(10) 0.31500(11) 0.11222(9) 0.0462(5) Uani 1 1 d . . . . .
H31 H 1.0293 0.2986 0.0972 0.055 Uiso 1 1 calc R U . . .
C32 C 0.98201(12) 0.37611(12) 0.13313(10) 0.0549(6) Uani 1 1 d . . . . .
H32 H 1.0251 0.4018 0.1329 0.066 Uiso 1 1 calc R U . . .
C33 C 0.91678(13) 0.40010(11) 0.15440(12) 0.0609(6) Uani 1 1 d . . . . .
H33 H 0.9150 0.4423 0.1689 0.073 Uiso 1 1 calc R U . . .
C34 C 0.85375(12) 0.36255(9) 0.15467(11) 0.0496(5) Uani 1 1 d . . . . .
H34 H 0.8089 0.3795 0.1689 0.059 Uiso 1 1 calc R U . . .
C35 C 0.73012(9) 0.27275(8) 0.20235(7) 0.0311(3) Uani 1 1 d . . . . .
C36 C 0.74987(10) 0.24395(9) 0.25312(8) 0.0376(4) Uani 1 1 d . . . . .
H36 H 0.7852 0.2105 0.2530 0.045 Uiso 1 1 calc R U . . .
C37 C 0.71863(11) 0.26340(10) 0.30418(8) 0.0445(4) Uani 1 1 d . . . . .
H37 H 0.7332 0.2438 0.3387 0.053 Uiso 1 1 calc R U . . .
C38 C 0.66643(11) 0.31127(9) 0.30462(8) 0.0430(4) Uani 1 1 d . . . . .
H38 H 0.6452 0.3248 0.3395 0.052 Uiso 1 1 calc R U . . .
C39 C 0.64518(10) 0.33939(9) 0.25416(9) 0.0425(4) Uani 1 1 d . . . . .
H39 H 0.6086 0.3717 0.2543 0.051 Uiso 1 1 calc R U . . .
C40 C 0.67684(9) 0.32075(9) 0.20338(8) 0.0372(4) Uani 1 1 d . . . . .
H40 H 0.6623 0.3407 0.1690 0.045 Uiso 1 1 calc R U . . .
C41 C 0.71527(9) 0.27570(8) 0.08142(7) 0.0313(3) Uani 1 1 d . . . . .
C42 C 0.64264(10) 0.25369(9) 0.07967(8) 0.0404(4) Uani 1 1 d . . . . .
H42 H 0.6244 0.2278 0.1096 0.049 Uiso 1 1 calc R U . . .
C43 C 0.59684(11) 0.26939(10) 0.03438(9) 0.0479(5) Uani 1 1 d . . . . .
H43 H 0.5475 0.2545 0.0339 0.058 Uiso 1 1 calc R U . . .
C44 C 0.62242(12) 0.30626(10) -0.00956(9) 0.0493(5) Uani 1 1 d . . . . .
H44 H 0.5909 0.3167 -0.0404 0.059 Uiso 1 1 calc R U . . .
C45 C 0.69399(12) 0.32794(11) -0.00864(9) 0.0502(5) Uani 1 1 d . . . . .
H45 H 0.7121 0.3531 -0.0391 0.060 Uiso 1 1 calc R U . . .
C46 C 0.73985(10) 0.31302(9) 0.03686(8) 0.0401(4) Uani 1 1 d . . . . .
H46 H 0.7889 0.3288 0.0373 0.048 Uiso 1 1 calc R U . . .
N1 N 0.84798(7) 0.06138(7) 0.27442(5) 0.0284(3) Uani 1 1 d . . . . .
N2 N 0.94772(7) 0.10907(7) 0.25215(5) 0.0289(3) Uani 1 1 d . . . . .
N3 N 0.91629(7) 0.00990(7) 0.17651(5) 0.0298(3) Uani 1 1 d . . . . .
P1 P 0.81031(2) 0.06654(2) 0.06329(2) 0.02714(9) Uani 1 1 d . . . . .
P2 P 0.77694(2) 0.24542(2) 0.13743(2) 0.02769(9) Uani 1 1 d . . . . .
Pd1 Pd 0.81616(2) 0.14190(2) 0.13465(2) 0.02494(5) Uani 1 1 d . . . . .
Si1 Si 0.87579(2) 0.08342(2) 0.20093(2) 0.02556(9) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C4 1.528(2) . ?
C2 C4 1.522(2) . ?
C3 C4 1.524(2) . ?
C4 N1 1.476(2) . ?
C5 N1 1.337(2) . ?
C5 N2 1.338(2) . ?
C5 C6 1.489(2) . ?
C5 Si1 2.3143(15) . ?
C6 C7 1.384(3) . ?
C6 C11 1.385(3) . ?
C7 C8 1.391(3) . ?
C8 C9 1.370(4) . ?
C9 C10 1.369(4) . ?
C10 C11 1.390(3) . ?
C12 N2 1.483(2) . ?
C12 C14 1.522(3) . ?
C12 C13 1.526(3) . ?
C12 C15 1.532(2) . ?
C16 C17 1.362(3) . ?
C16 N3 1.390(2) . ?
C17 C18 1.411(3) . ?
C18 C19 1.370(3) . ?
C19 N3 1.393(2) . ?
C19 C20 1.499(2) . ?
C20 P1 1.8658(18) . ?
C21 C24 1.530(3) . ?
C21 C23 1.531(2) . ?
C21 C22 1.539(2) . ?
C21 P1 1.8850(17) . ?
C25 C28 1.524(3) . ?
C25 C27 1.534(3) . ?
C25 C26 1.540(3) . ?
C25 P1 1.8949(18) . ?
C29 C34 1.388(3) . ?
C29 C30 1.388(3) . ?
C29 P2 1.8418(18) . ?
C30 C31 1.385(3) . ?
C31 C32 1.375(3) . ?
C32 C33 1.381(4) . ?
C33 C34 1.390(3) . ?
C35 C36 1.387(2) . ?
C35 C40 1.397(2) . ?
C35 P2 1.8413(17) . ?
C36 C37 1.391(3) . ?
C37 C38 1.381(3) . ?
C38 C39 1.382(3) . ?
C39 C40 1.384(3) . ?
C41 C46 1.384(3) . ?
C41 C42 1.398(3) . ?
C41 P2 1.8434(17) . ?
C42 C43 1.392(3) . ?
C43 C44 1.373(3) . ?
C44 C45 1.377(3) . ?
C45 C46 1.393(3) . ?
N1 Si1 1.8615(13) . ?
N2 Si1 1.8579(13) . ?
N3 Si1 1.8041(14) . ?
P1 Pd1 2.3108(4) . ?
P2 Pd1 2.2881(4) . ?
Pd1 Si1 2.2622(4) . ?

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
N1 C4 C2 111.79(14) . . ?
N1 C4 C3 109.95(14) . . ?
C2 C4 C3 110.59(15) . . ?
N1 C4 C1 105.50(13) . . ?
C2 C4 C1 109.46(15) . . ?
C3 C4 C1 109.42(15) . . ?
N1 C5 N2 105.92(13) . . ?
N1 C5 C6 126.57(14) . . ?
N2 C5 C6 127.37(14) . . ?
N1 C5 Si1 53.53(8) . . ?
N2 C5 Si1 53.38(8) . . ?
C6 C5 Si1 168.05(13) . . ?
C7 C6 C11 119.72(17) . . ?
C7 C6 C5 119.83(17) . . ?
C11 C6 C5 120.44(17) . . ?
C6 C7 C8 119.9(2) . . ?
C9 C8 C7 120.1(2) . . ?
C10 C9 C8 120.4(2) . . ?
C9 C10 C11 120.3(2) . . ?
C6 C11 C10 119.7(2) . . ?
N2 C12 C14 110.58(15) . . ?
N2 C12 C13 111.00(15) . . ?
C14 C12 C13 111.13(17) . . ?
N2 C12 C15 105.16(14) . . ?
C14 C12 C15 109.27(16) . . ?
C13 C12 C15 109.52(16) . . ?
C17 C16 N3 109.90(16) . . ?
C16 C17 C18 106.81(16) . . ?
C19 C18 C17 108.11(16) . . ?
C18 C19 N3 108.60(15) . . ?
C18 C19 C20 125.70(16) . . ?
N3 C19 C20 125.43(15) . . ?
C19 C20 P1 120.56(12) . . ?
C24 C21 C23 109.99(16) . . ?
C24 C21 C22 106.76(16) . . ?
C23 C21 C22 109.57(15) . . ?
C24 C21 P1 109.78(13) . . ?
C23 C21 P1 115.30(13) . . ?
C22 C21 P1 105.00(11) . . ?
C28 C25 C27 109.93(16) . . ?
C28 C25 C26 108.73(17) . . ?
C27 C25 C26 107.69(17) . . ?
C28 C25 P1 116.35(14) . . ?
C27 C25 P1 109.68(13) . . ?
C26 C25 P1 104.01(12) . . ?
C34 C29 C30 118.26(17) . . ?
C34 C29 P2 123.74(15) . . ?
C30 C29 P2 117.90(14) . . ?
C31 C30 C29 121.31(18) . . ?
C32 C31 C30 119.74(19) . . ?
C31 C32 C33 120.00(19) . . ?
C32 C33 C34 120.1(2) . . ?
C29 C34 C33 120.6(2) . . ?
C36 C35 C40 118.59(16) . . ?
C36 C35 P2 117.45(13) . . ?
C40 C35 P2 123.97(13) . . ?
C35 C36 C37 120.80(17) . . ?
C38 C37 C36 120.00(18) . . ?
C37 C38 C39 119.72(17) . . ?
C38 C39 C40 120.45(17) . . ?
C39 C40 C35 120.43(18) . . ?
C46 C41 C42 117.97(16) . . ?
C46 C41 P2 122.83(13) . . ?
C42 C41 P2 118.70(13) . . ?
C43 C42 C41 120.53(18) . . ?
C44 C43 C42 120.58(18) . . ?
C43 C44 C45 119.59(18) . . ?
C44 C45 C46 120.1(2) . . ?
C41 C46 C45 121.20(18) . . ?
C5 N1 C4 131.87(13) . . ?
C5 N1 Si1 91.19(10) . . ?
C4 N1 Si1 136.31(10) . . ?
C5 N2 C12 130.37(14) . . ?
C5 N2 Si1 91.32(9) . . ?
C12 N2 Si1 133.37(11) . . ?
C16 N3 C19 106.58(14) . . ?
C16 N3 Si1 125.91(12) . . ?
C19 N3 Si1 127.42(11) . . ?
C20 P1 C21 104.13(8) . . ?
C20 P1 C25 98.98(8) . . ?
C21 P1 C25 111.30(8) . . ?
C20 P1 Pd1 109.89(5) . . ?
C21 P1 Pd1 117.46(6) . . ?
C25 P1 Pd1 113.04(6) . . ?
C35 P2 C29 101.31(8) . . ?
C35 P2 C41 101.92(8) . . ?
C29 P2 C41 103.10(7) . . ?
C35 P2 Pd1 117.61(6) . . ?
C29 P2 Pd1 110.73(6) . . ?
C41 P2 Pd1 119.74(5) . . ?
Si1 Pd1 P2 130.147(15) . . ?
Si1 Pd1 P1 98.769(15) . . ?
P2 Pd1 P1 131.063(15) . . ?
N3 Si1 N2 99.70(6) . . ?
N3 Si1 N1 101.21(6) . . ?
N2 Si1 N1 70.06(6) . . ?
N3 Si1 Pd1 116.06(5) . . ?
N2 Si1 Pd1 128.86(5) . . ?
N1 Si1 Pd1 130.31(5) . . ?
N3 Si1 C5 107.38(6) . . ?
N2 Si1 C5 35.30(6) . . ?
N1 Si1 C5 35.28(6) . . ?
Pd1 Si1 C5 136.51(4) . . ?

_refine_diff_density_max         0.268
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.053

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_3Ni-Ge
_database_code_depnum_ccdc_archive 'CCDC 2001502'
loop_
_audit_author_name
_audit_author_address
'Javier A. Cabeza'
;Universidad de Oviedo
Spain
;
_audit_update_record             
;
2020-05-06 deposited with the CCDC.	2020-06-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H58 Ge N3 Ni P'
_chemical_formula_sum            'C36 H58 Ge N3 Ni P'
_chemical_formula_weight         695.12

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'
Ge Ge 0.1547 1.8001 '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'
Ni Ni 0.3393 1.1124 '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'

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

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

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

_cell_length_a                   20.5915(11)
_cell_length_b                   8.8479(3)
_cell_length_c                   20.8528(8)
_cell_angle_alpha                90
_cell_angle_beta                 109.118(5)
_cell_angle_gamma                90
_cell_volume                     3589.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4847
_cell_measurement_theta_min      2.5870
_cell_measurement_theta_max      22.6230

_exptl_crystal_description       fragment
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_F_000             1480
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    1.434
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   multi-scan
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.78012
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            51967
_diffrn_reflns_av_unetI/netI     0.2034
_diffrn_reflns_av_R_equivalents  0.1668
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.413
_diffrn_reflns_theta_max         31.443
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11120
_reflns_number_gt                5388
_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       
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_cell_refinement       
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction        
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_structure_solution    'SIR-97 (Giacovazzo, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    
'MERCURY (Cambridge Crystallographic Data Centre: Cambridge, UK, 2018)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'

_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)+(0.0017P)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_number_reflns         11120
_refine_ls_number_parameters     391
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1865
_refine_ls_R_factor_gt           0.0747
_refine_ls_wR_factor_ref         0.1084
_refine_ls_wR_factor_gt          0.0798
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7565(3) 0.0257(5) 0.2276(2) 0.0410(13) Uani 1 1 d . . . . .
H1A H 0.7880 0.0972 0.2584 0.062 Uiso 1 1 calc R U . . .
H1B H 0.7430 -0.0523 0.2541 0.062 Uiso 1 1 calc R U . . .
H1C H 0.7155 0.0797 0.1995 0.062 Uiso 1 1 calc R U . . .
C2 C 0.7448(2) -0.1675(5) 0.13645(18) 0.0354(12) Uani 1 1 d . . . . .
H2A H 0.7019 -0.1192 0.1090 0.053 Uiso 1 1 calc R U . . .
H2B H 0.7347 -0.2462 0.1649 0.053 Uiso 1 1 calc R U . . .
H2C H 0.7675 -0.2130 0.1065 0.053 Uiso 1 1 calc R U . . .
C3 C 0.8581(2) -0.1270(5) 0.2257(2) 0.0447(14) Uani 1 1 d . . . . .
H3A H 0.8840 -0.1636 0.1968 0.067 Uiso 1 1 calc R U . . .
H3B H 0.8461 -0.2126 0.2495 0.067 Uiso 1 1 calc R U . . .
H3C H 0.8864 -0.0551 0.2590 0.067 Uiso 1 1 calc R U . . .
C4 C 0.7924(2) -0.0486(4) 0.18186(18) 0.0249(10) Uani 1 1 d . . . . .
C5 C 0.8479(2) 0.1812(5) 0.14579(18) 0.0226(10) Uani 1 1 d . . . . .
C6 C 0.8856(2) 0.2485(5) 0.21351(18) 0.0245(10) Uani 1 1 d . . . . .
C7 C 0.8545(2) 0.3655(5) 0.23754(18) 0.0268(10) Uani 1 1 d . . . . .
H7 H 0.8108 0.4018 0.2102 0.032 Uiso 1 1 calc R U . . .
C8 C 0.8865(2) 0.4297(5) 0.30083(19) 0.0347(12) Uani 1 1 d . . . . .
H8 H 0.8650 0.5103 0.3163 0.042 Uiso 1 1 calc R U . . .
C9 C 0.9495(2) 0.3760(5) 0.3411(2) 0.0373(13) Uani 1 1 d . . . . .
H9 H 0.9710 0.4175 0.3849 0.045 Uiso 1 1 calc R U . . .
C10 C 0.9813(2) 0.2622(6) 0.3177(2) 0.0399(13) Uani 1 1 d . . . . .
H10 H 1.0251 0.2267 0.3453 0.048 Uiso 1 1 calc R U . . .
C11 C 0.9500(2) 0.1984(5) 0.25397(18) 0.0309(11) Uani 1 1 d . . . . .
H11 H 0.9726 0.1206 0.2381 0.037 Uiso 1 1 calc R U . . .
C12 C 0.8816(2) 0.3727(5) 0.06926(18) 0.0258(10) Uani 1 1 d . . . . .
C13 C 0.8505(2) 0.5212(5) 0.08377(19) 0.0323(11) Uani 1 1 d . . . . .
H13A H 0.8004 0.5171 0.0636 0.048 Uiso 1 1 calc R U . . .
H13B H 0.8682 0.6057 0.0640 0.048 Uiso 1 1 calc R U . . .
H13C H 0.8631 0.5356 0.1329 0.048 Uiso 1 1 calc R U . . .
C14 C 0.9587(2) 0.3670(5) 0.10746(19) 0.0365(12) Uani 1 1 d . . . . .
H14A H 0.9668 0.3782 0.1562 0.055 Uiso 1 1 calc R U . . .
H14B H 0.9816 0.4493 0.0918 0.055 Uiso 1 1 calc R U . . .
H14C H 0.9772 0.2699 0.0989 0.055 Uiso 1 1 calc R U . . .
C15 C 0.8699(2) 0.3618(5) -0.00738(17) 0.0346(12) Uani 1 1 d . . . . .
H15A H 0.8894 0.2669 -0.0171 0.052 Uiso 1 1 calc R U . . .
H15B H 0.8923 0.4473 -0.0215 0.052 Uiso 1 1 calc R U . . .
H15C H 0.8205 0.3643 -0.0324 0.052 Uiso 1 1 calc R U . . .
C16 C 0.8909(2) -0.0465(5) 0.0195(2) 0.0304(11) Uani 1 1 d . . . . .
H16 H 0.9231 0.0132 0.0530 0.036 Uiso 1 1 calc R U . . .
C17 C 0.9076(2) -0.1500(5) -0.02112(19) 0.0320(11) Uani 1 1 d . . . . .
H17 H 0.9525 -0.1748 -0.0211 0.038 Uiso 1 1 calc R U . . .
C18 C 0.8451(2) -0.2129(5) -0.06313(18) 0.0284(11) Uani 1 1 d . . . . .
H18 H 0.8401 -0.2882 -0.0969 0.034 Uiso 1 1 calc R U . . .
C19 C 0.7927(2) -0.1453(4) -0.04627(17) 0.0212(10) Uani 1 1 d . . . . .
C20 C 0.7177(2) -0.1804(4) -0.07033(17) 0.0238(10) Uani 1 1 d . . . . .
H20A H 0.7064 -0.2251 -0.0317 0.029 Uiso 1 1 calc R U . . .
H20B H 0.7096 -0.2597 -0.1056 0.029 Uiso 1 1 calc R U . . .
C21 C 0.6796(2) 0.0371(5) -0.18197(17) 0.0236(10) Uani 1 1 d . . . . .
C22 C 0.7043(2) -0.0885(5) -0.21966(18) 0.0326(11) Uani 1 1 d . . . . .
H22A H 0.6674 -0.1623 -0.2378 0.049 Uiso 1 1 calc R U . . .
H22B H 0.7445 -0.1390 -0.1881 0.049 Uiso 1 1 calc R U . . .
H22C H 0.7168 -0.0441 -0.2570 0.049 Uiso 1 1 calc R U . . .
C23 C 0.7391(2) 0.1510(4) -0.15484(18) 0.0278(11) Uani 1 1 d . . . . .
H23A H 0.7530 0.1886 -0.1926 0.042 Uiso 1 1 calc R U . . .
H23B H 0.7782 0.1009 -0.1216 0.042 Uiso 1 1 calc R U . . .
H23C H 0.7238 0.2359 -0.1332 0.042 Uiso 1 1 calc R U . . .
C24 C 0.6192(2) 0.1204(5) -0.23348(17) 0.0307(11) Uani 1 1 d . . . . .
H24A H 0.6362 0.1784 -0.2648 0.046 Uiso 1 1 calc R U . . .
H24B H 0.5980 0.1892 -0.2093 0.046 Uiso 1 1 calc R U . . .
H24C H 0.5851 0.0466 -0.2592 0.046 Uiso 1 1 calc R U . . .
C25 C 0.5737(2) -0.1436(5) -0.13723(17) 0.0252(10) Uani 1 1 d . . . . .
C26 C 0.5695(2) -0.2318(4) -0.07490(18) 0.0298(11) Uani 1 1 d . . . . .
H26A H 0.5854 -0.1673 -0.0346 0.045 Uiso 1 1 calc R U . . .
H26B H 0.5986 -0.3220 -0.0681 0.045 Uiso 1 1 calc R U . . .
H26C H 0.5218 -0.2622 -0.0824 0.045 Uiso 1 1 calc R U . . .
C27 C 0.5709(2) -0.2615(5) -0.19271(18) 0.0345(12) Uani 1 1 d . . . . .
H27A H 0.5322 -0.3302 -0.1981 0.052 Uiso 1 1 calc R U . . .
H27B H 0.6138 -0.3195 -0.1794 0.052 Uiso 1 1 calc R U . . .
H27C H 0.5651 -0.2097 -0.2358 0.052 Uiso 1 1 calc R U . . .
C28 C 0.5094(2) -0.0433(5) -0.16314(19) 0.0300(11) Uani 1 1 d . . . . .
H28A H 0.4681 -0.1065 -0.1741 0.045 Uiso 1 1 calc R U . . .
H28B H 0.5100 0.0108 -0.2039 0.045 Uiso 1 1 calc R U . . .
H28C H 0.5091 0.0298 -0.1279 0.045 Uiso 1 1 calc R U . . .
C29 C 0.6177(2) 0.3519(4) -0.08663(17) 0.0233(10) Uani 1 1 d . . . . .
H29 H 0.6350 0.3214 -0.1216 0.028 Uiso 1 1 calc R U . . .
C30 C 0.6652(2) 0.3949(4) -0.02512(17) 0.0226(9) Uani 1 1 d . . . . .
H30 H 0.7126 0.3881 -0.0203 0.027 Uiso 1 1 calc R U . . .
C31 C 0.6460(2) 0.4523(5) 0.03544(18) 0.0287(11) Uani 1 1 d . . . . .
H31A H 0.6005 0.5023 0.0185 0.034 Uiso 1 1 calc R U . . .
H31B H 0.6800 0.5293 0.0598 0.034 Uiso 1 1 calc R U . . .
C32 C 0.6432(2) 0.3274(5) 0.08559(18) 0.0306(11) Uani 1 1 d . . . . .
H32A H 0.6895 0.3157 0.1198 0.037 Uiso 1 1 calc R U . . .
H32B H 0.6113 0.3587 0.1098 0.037 Uiso 1 1 calc R U . . .
C33 C 0.6201(2) 0.1762(5) 0.05176(18) 0.0271(10) Uani 1 1 d . . . . .
H33 H 0.6455 0.0896 0.0727 0.032 Uiso 1 1 calc R U . . .
C34 C 0.5651(2) 0.1531(5) -0.00702(18) 0.0268(10) Uani 1 1 d . . . . .
H34 H 0.5561 0.0528 -0.0239 0.032 Uiso 1 1 calc R U . . .
C35 C 0.5182(2) 0.2781(5) -0.04607(18) 0.0285(11) Uani 1 1 d . . . . .
H35A H 0.5158 0.3581 -0.0137 0.034 Uiso 1 1 calc R U . . .
H35B H 0.4713 0.2365 -0.0667 0.034 Uiso 1 1 calc R U . . .
C36 C 0.5410(2) 0.3498(5) -0.10229(17) 0.0253(10) Uani 1 1 d . . . . .
H36A H 0.5199 0.2931 -0.1450 0.030 Uiso 1 1 calc R U . . .
H36B H 0.5236 0.4548 -0.1098 0.030 Uiso 1 1 calc R U . . .
Ge1 Ge 0.76774(2) 0.10382(5) 0.03483(2) 0.02088(11) Uani 1 1 d . . . . .
N1 N 0.80689(17) 0.0609(4) 0.13498(14) 0.0230(8) Uani 1 1 d . . . . .
N2 N 0.84587(17) 0.2387(4) 0.08553(14) 0.0234(8) Uani 1 1 d . . . . .
N3 N 0.82090(17) -0.0413(4) 0.00481(14) 0.0220(8) Uani 1 1 d . . . . .
Ni1 Ni 0.65930(3) 0.15450(6) -0.02992(2) 0.02050(14) Uani 1 1 d . . . . .
P1 P 0.65481(6) -0.02479(12) -0.10590(5) 0.0204(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C4 1.533(5) . ?
C2 C4 1.535(5) . ?
C3 C4 1.529(5) . ?
C4 N1 1.474(5) . ?
C5 N1 1.330(5) . ?
C5 N2 1.344(4) . ?
C5 C6 1.495(5) . ?
C5 Ge1 2.458(4) . ?
C6 C11 1.391(5) . ?
C6 C7 1.393(5) . ?
C7 C8 1.389(5) . ?
C8 C9 1.380(6) . ?
C9 C10 1.374(6) . ?
C10 C11 1.392(5) . ?
C12 N2 1.492(5) . ?
C12 C14 1.526(5) . ?
C12 C13 1.534(5) . ?
C12 C15 1.539(5) . ?
C16 C17 1.365(5) . ?
C16 N3 1.373(5) . ?
C17 C18 1.413(6) . ?
C18 C19 1.376(5) . ?
C19 N3 1.383(4) . ?
C19 C20 1.491(5) . ?
C20 P1 1.869(4) . ?
C21 C24 1.539(5) . ?
C21 C22 1.541(5) . ?
C21 C23 1.544(5) . ?
C21 P1 1.899(4) . ?
C25 C28 1.537(5) . ?
C25 C26 1.543(5) . ?
C25 C27 1.545(5) . ?
C25 P1 1.900(4) . ?
C29 C30 1.387(5) . ?
C29 C36 1.503(5) . ?
C29 Ni1 2.126(4) . ?
C30 C31 1.528(5) . ?
C30 Ni1 2.131(4) . ?
C31 C32 1.536(5) . ?
C32 C33 1.515(5) . ?
C33 C34 1.385(5) . ?
C33 Ni1 2.119(4) . ?
C34 C35 1.517(5) . ?
C34 Ni1 2.145(4) . ?
C35 C36 1.536(5) . ?
Ge1 N3 1.921(3) . ?
Ge1 N2 2.004(3) . ?
Ge1 N1 2.013(3) . ?
Ge1 Ni1 2.2439(7) . ?
Ni1 P1 2.2224(11) . ?

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
N1 C4 C3 111.4(4) . . ?
N1 C4 C1 112.0(3) . . ?
C3 C4 C1 109.6(3) . . ?
N1 C4 C2 105.6(3) . . ?
C3 C4 C2 108.6(3) . . ?
C1 C4 C2 109.7(4) . . ?
N1 C5 N2 108.7(3) . . ?
N1 C5 C6 125.7(4) . . ?
N2 C5 C6 125.5(4) . . ?
N1 C5 Ge1 54.90(18) . . ?
N2 C5 Ge1 54.54(19) . . ?
C6 C5 Ge1 168.9(3) . . ?
C11 C6 C7 118.5(4) . . ?
C11 C6 C5 122.9(4) . . ?
C7 C6 C5 118.6(4) . . ?
C8 C7 C6 121.0(4) . . ?
C9 C8 C7 119.7(4) . . ?
C10 C9 C8 120.0(4) . . ?
C9 C10 C11 120.7(4) . . ?
C6 C11 C10 120.1(4) . . ?
N2 C12 C14 111.2(3) . . ?
N2 C12 C13 111.5(3) . . ?
C14 C12 C13 110.8(3) . . ?
N2 C12 C15 105.3(3) . . ?
C14 C12 C15 108.8(4) . . ?
C13 C12 C15 109.0(3) . . ?
C17 C16 N3 110.1(4) . . ?
C16 C17 C18 106.6(4) . . ?
C19 C18 C17 107.6(4) . . ?
C18 C19 N3 108.6(4) . . ?
C18 C19 C20 129.5(4) . . ?
N3 C19 C20 121.7(4) . . ?
C19 C20 P1 119.1(3) . . ?
C24 C21 C22 108.4(3) . . ?
C24 C21 C23 107.8(3) . . ?
C22 C21 C23 107.6(3) . . ?
C24 C21 P1 110.2(3) . . ?
C22 C21 P1 116.3(3) . . ?
C23 C21 P1 106.3(2) . . ?
C28 C25 C26 108.0(3) . . ?
C28 C25 C27 108.1(3) . . ?
C26 C25 C27 106.9(3) . . ?
C28 C25 P1 111.1(3) . . ?
C26 C25 P1 106.0(2) . . ?
C27 C25 P1 116.3(3) . . ?
C30 C29 C36 125.2(4) . . ?
C30 C29 Ni1 71.2(2) . . ?
C36 C29 Ni1 108.3(3) . . ?
C29 C30 C31 124.1(4) . . ?
C29 C30 Ni1 70.8(2) . . ?
C31 C30 Ni1 110.2(3) . . ?
C30 C31 C32 113.6(3) . . ?
C33 C32 C31 113.3(3) . . ?
C34 C33 C32 125.7(4) . . ?
C34 C33 Ni1 72.1(2) . . ?
C32 C33 Ni1 108.0(3) . . ?
C33 C34 C35 124.0(4) . . ?
C33 C34 Ni1 70.0(2) . . ?
C35 C34 Ni1 109.8(3) . . ?
C34 C35 C36 114.3(3) . . ?
C29 C36 C35 113.7(3) . . ?
N3 Ge1 N2 97.21(14) . . ?
N3 Ge1 N1 97.74(13) . . ?
N2 Ge1 N1 65.50(12) . . ?
N3 Ge1 Ni1 119.91(9) . . ?
N2 Ge1 Ni1 131.85(10) . . ?
N1 Ge1 Ni1 130.04(10) . . ?
N3 Ge1 C5 102.39(13) . . ?
N2 Ge1 C5 33.10(12) . . ?
N1 Ge1 C5 32.73(12) . . ?
Ni1 Ge1 C5 137.68(10) . . ?
C5 N1 C4 131.9(3) . . ?
C5 N1 Ge1 92.4(2) . . ?
C4 N1 Ge1 135.4(3) . . ?
C5 N2 C12 130.3(3) . . ?
C5 N2 Ge1 92.4(3) . . ?
C12 N2 Ge1 136.4(2) . . ?
C16 N3 C19 107.2(3) . . ?
C16 N3 Ge1 128.2(3) . . ?
C19 N3 Ge1 123.7(3) . . ?
C33 Ni1 C29 100.51(16) . . ?
C33 Ni1 C30 84.40(15) . . ?
C29 Ni1 C30 38.04(13) . . ?
C33 Ni1 C34 37.90(14) . . ?
C29 Ni1 C34 84.22(16) . . ?
C30 Ni1 C34 92.11(16) . . ?
C33 Ni1 P1 134.40(12) . . ?
C29 Ni1 P1 105.96(10) . . ?
C30 Ni1 P1 137.27(10) . . ?
C34 Ni1 P1 108.97(11) . . ?
C33 Ni1 Ge1 95.77(11) . . ?
C29 Ni1 Ge1 129.74(11) . . ?
C30 Ni1 Ge1 98.13(11) . . ?
C34 Ni1 Ge1 131.25(10) . . ?
P1 Ni1 Ge1 95.00(4) . . ?
C20 P1 C21 101.72(19) . . ?
C20 P1 C25 98.39(18) . . ?
C21 P1 C25 108.60(17) . . ?
C20 P1 Ni1 112.41(12) . . ?
C21 P1 Ni1 115.46(13) . . ?
C25 P1 Ni1 117.81(14) . . ?

_refine_diff_density_max         0.766
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.128

_shelxl_version_number           2014-3

