# Electronic Supplementary Material (ESI) for ChemComm.
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 2035174'
loop_
_audit_author_name
_audit_author_address
'Javier A. Cabeza'
;Universidad de Oviedo
Spain
;
_audit_update_record             
;
2020-10-02 deposited with the CCDC.	2020-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H42 Cl2 Ge N2 P2 Pd'
_chemical_formula_sum            'C25 H42 Cl2 Ge N2 P2 Pd'
_chemical_formula_weight         682.43

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'
Ge Ge -1.0885 0.8855 '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'

_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                   11.4960(2)
_cell_length_b                   18.4130(3)
_cell_length_c                   14.6710(3)
_cell_angle_alpha                90
_cell_angle_beta                 106.665(2)
_cell_angle_gamma                90
_cell_volume                     2975.06(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    140(2)
_cell_measurement_reflns_used    11320
_cell_measurement_theta_min      3.9980
_cell_measurement_theta_max      69.4910

_exptl_crystal_description       fragment
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_F_000             1392
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    8.908
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.23726
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      140(2)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16009
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.957
_diffrn_reflns_theta_max         69.641
_diffrn_reflns_theta_full        67.680
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5525
_reflns_number_gt                5074
_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 1.171.38.43 (Rigaku Oxford Diffraction, 2015)'
_computing_cell_refinement       
'CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction        
'CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)'
_computing_structure_solution    'SIR-97 (Giacovazzo, 1999)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    
'MERCURY (Cambridge Crystallographic Data Centre: Cambridge, UK, 2020)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'

_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)+(0.0612P)²+1.1646P] 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         5525
_refine_ls_number_parameters     308
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0363
_refine_ls_wR_factor_ref         0.0998
_refine_ls_wR_factor_gt          0.0957
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_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 0.3854(5) 0.2668(3) 0.1671(6) 0.109(2) Uani 1 1 d . . . . .
H1A H 0.3108 0.2954 0.1440 0.163 Uiso 1 1 calc R U . . .
H1B H 0.4112 0.2495 0.1128 0.163 Uiso 1 1 calc R U . . .
H1C H 0.4493 0.2972 0.2079 0.163 Uiso 1 1 calc R U . . .
C2 C 0.3643(6) 0.2243(4) 0.3223(5) 0.114(2) Uani 1 1 d . . . . .
H2A H 0.4427 0.2470 0.3539 0.170 Uiso 1 1 calc R U . . .
H2B H 0.3532 0.1814 0.3584 0.170 Uiso 1 1 calc R U . . .
H2C H 0.2988 0.2591 0.3194 0.170 Uiso 1 1 calc R U . . .
C3 C 0.3617(4) 0.2023(2) 0.2239(4) 0.0677(13) Uani 1 1 d . . . . .
H3 H 0.4311 0.1680 0.2305 0.081 Uiso 1 1 calc R U . . .
C4 C 0.1373(5) 0.0524(2) 0.0239(3) 0.0592(10) Uani 1 1 d . . . . .
H4A H 0.0559 0.0729 0.0138 0.089 Uiso 1 1 calc R U . . .
H4B H 0.1517 0.0151 0.0735 0.089 Uiso 1 1 calc R U . . .
H4C H 0.1436 0.0307 -0.0354 0.089 Uiso 1 1 calc R U . . .
C5 C 0.2261(8) 0.1653(3) -0.0221(5) 0.109(2) Uani 1 1 d . . . . .
H5A H 0.2333 0.1396 -0.0787 0.163 Uiso 1 1 calc R U . . .
H5B H 0.2928 0.2002 -0.0011 0.163 Uiso 1 1 calc R U . . .
H5C H 0.1484 0.1912 -0.0375 0.163 Uiso 1 1 calc R U . . .
C6 C 0.2316(4) 0.1124(2) 0.0548(3) 0.0641(11) Uani 1 1 d . . . . .
H6 H 0.3127 0.0883 0.0686 0.077 Uiso 1 1 calc R U . . .
C7 C 0.0988(3) 0.21884(18) 0.1428(3) 0.0456(8) Uani 1 1 d . . . . .
H7A H 0.1053 0.2472 0.2014 0.055 Uiso 1 1 calc R U . . .
H7B H 0.1117 0.2529 0.0943 0.055 Uiso 1 1 calc R U . . .
C8 C -0.0269(3) 0.18875(18) 0.1078(3) 0.0433(7) Uani 1 1 d . . . . .
C9 C -0.1139(3) 0.1979(2) 0.0236(3) 0.0490(8) Uani 1 1 d . . . . .
H9 H -0.1068 0.2265 -0.0284 0.059 Uiso 1 1 calc R U . . .
C10 C -0.2175(3) 0.1570(2) 0.0271(3) 0.0495(8) Uani 1 1 d . . . . .
H10 H -0.2916 0.1531 -0.0224 0.059 Uiso 1 1 calc R U . . .
C11 C -0.1914(3) 0.12414(18) 0.1146(2) 0.0397(7) Uani 1 1 d . . . . .
C12 C -0.2734(3) 0.08241(18) 0.1600(2) 0.0400(7) Uani 1 1 d . . . . .
C13 C -0.3229(3) 0.13576(19) 0.2207(3) 0.0479(8) Uani 1 1 d . . . . .
H13A H -0.2553 0.1557 0.2713 0.072 Uiso 1 1 calc R U . . .
H13B H -0.3788 0.1101 0.2490 0.072 Uiso 1 1 calc R U . . .
H13C H -0.3662 0.1754 0.1804 0.072 Uiso 1 1 calc R U . . .
C14 C -0.3816(3) 0.0510(2) 0.0828(3) 0.0560(10) Uani 1 1 d . . . . .
H14A H -0.4272 0.0906 0.0440 0.084 Uiso 1 1 calc R U . . .
H14B H -0.4348 0.0245 0.1129 0.084 Uiso 1 1 calc R U . . .
H14C H -0.3519 0.0177 0.0423 0.084 Uiso 1 1 calc R U . . .
C15 C -0.2101(2) 0.02142(18) 0.2249(2) 0.0370(7) Uani 1 1 d . . . . .
C16 C -0.2541(3) -0.04172(18) 0.2494(3) 0.0447(8) Uani 1 1 d . . . . .
H16 H -0.3331 -0.0608 0.2214 0.054 Uiso 1 1 calc R U . . .
C17 C -0.1616(3) -0.07452(19) 0.3241(3) 0.0452(7) Uani 1 1 d . . . . .
H17 H -0.1674 -0.1193 0.3547 0.054 Uiso 1 1 calc R U . . .
C18 C -0.0636(3) -0.02989(17) 0.3434(2) 0.0367(6) Uani 1 1 d . . . . .
C19 C 0.0595(3) -0.0384(2) 0.4138(2) 0.0413(7) Uani 1 1 d . . . . .
H19A H 0.0595 -0.0831 0.4513 0.050 Uiso 1 1 calc R U . . .
H19B H 0.0737 0.0032 0.4584 0.050 Uiso 1 1 calc R U . . .
C20 C 0.1644(4) -0.1320(2) 0.3000(3) 0.0587(10) Uani 1 1 d . . . . .
H20 H 0.1344 -0.1669 0.3405 0.070 Uiso 1 1 calc R U . . .
C21 C 0.0673(5) -0.1260(2) 0.2050(3) 0.0665(11) Uani 1 1 d . . . . .
H21A H 0.0980 -0.0966 0.1612 0.100 Uiso 1 1 calc R U . . .
H21B H -0.0052 -0.1028 0.2144 0.100 Uiso 1 1 calc R U . . .
H21C H 0.0463 -0.1746 0.1782 0.100 Uiso 1 1 calc R U . . .
C22 C 0.2814(6) -0.1628(3) 0.2867(5) 0.098(2) Uani 1 1 d . . . . .
H22A H 0.2637 -0.2081 0.2504 0.147 Uiso 1 1 calc R U . . .
H22B H 0.3390 -0.1724 0.3491 0.147 Uiso 1 1 calc R U . . .
H22C H 0.3167 -0.1276 0.2521 0.147 Uiso 1 1 calc R U . . .
C23 C 0.3205(3) -0.0493(3) 0.4652(3) 0.0768(16) Uani 1 1 d . . . . .
H23 H 0.3913 -0.0615 0.4413 0.092 Uiso 1 1 calc R U . . .
C24 C 0.3460(4) 0.0253(5) 0.5123(4) 0.105(2) Uani 1 1 d . . . . .
H24A H 0.2756 0.0411 0.5322 0.158 Uiso 1 1 calc R U . . .
H24B H 0.3614 0.0604 0.4669 0.158 Uiso 1 1 calc R U . . .
H24C H 0.4174 0.0223 0.5681 0.158 Uiso 1 1 calc R U . . .
C25 C 0.3099(5) -0.1101(5) 0.5334(4) 0.130(3) Uani 1 1 d . . . . .
H25A H 0.3866 -0.1145 0.5840 0.194 Uiso 1 1 calc R U . . .
H25B H 0.2920 -0.1560 0.4985 0.194 Uiso 1 1 calc R U . . .
H25C H 0.2443 -0.0987 0.5615 0.194 Uiso 1 1 calc R U . . .
Cl1 Cl 0.03562(7) 0.17078(5) 0.39112(6) 0.0486(2) Uani 1 1 d . . . . .
Cl2 Cl 0.40093(7) 0.01240(5) 0.25694(6) 0.0500(2) Uani 1 1 d . . . . .
Ge1 Ge 0.02298(3) 0.09607(2) 0.27103(2) 0.03281(11) Uani 1 1 d . . . . .
N1 N -0.0740(2) 0.14394(15) 0.16554(19) 0.0386(6) Uani 1 1 d . . . . .
N2 N -0.0918(2) 0.02945(14) 0.28385(18) 0.0351(5) Uani 1 1 d . . . . .
P1 P 0.22188(7) 0.15011(5) 0.16886(7) 0.0434(2) Uani 1 1 d . . . . .
P2 P 0.18667(7) -0.04358(5) 0.36072(6) 0.0408(2) Uani 1 1 d . . . . .
Pd1 Pd 0.20884(2) 0.05314(2) 0.26577(2) 0.03576(10) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C3 1.520(8) . ?
C2 C3 1.493(8) . ?
C3 P1 1.848(4) . ?
C4 C6 1.522(6) . ?
C5 C6 1.479(7) . ?
C6 P1 1.844(4) . ?
C7 C8 1.495(5) . ?
C7 P1 1.854(3) . ?
C8 C9 1.358(5) . ?
C8 N1 1.398(4) . ?
C9 C10 1.423(5) . ?
C10 C11 1.372(5) . ?
C11 N1 1.391(4) . ?
C11 C12 1.511(4) . ?
C12 C15 1.517(5) . ?
C12 C14 1.535(5) . ?
C12 C13 1.540(5) . ?
C15 C16 1.357(5) . ?
C15 N2 1.394(4) . ?
C16 C17 1.425(5) . ?
C17 C18 1.357(5) . ?
C18 N2 1.378(4) . ?
C18 C19 1.502(4) . ?
C19 P2 1.845(3) . ?
C20 C21 1.519(7) . ?
C20 C22 1.523(6) . ?
C20 P2 1.838(4) . ?
C23 C24 1.528(9) . ?
C23 C25 1.530(8) . ?
C23 P2 1.837(4) . ?
Cl1 Ge1 2.2070(8) . ?
Cl2 Pd1 2.3707(7) . ?
Ge1 N2 1.851(2) . ?
Ge1 N1 1.851(3) . ?
Ge1 Pd1 2.3001(4) . ?
P1 Pd1 2.3138(9) . ?
P2 Pd1 2.3197(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C3 C1 111.1(5) . . ?
C2 C3 P1 109.7(3) . . ?
C1 C3 P1 115.9(4) . . ?
C5 C6 C4 112.3(5) . . ?
C5 C6 P1 116.4(4) . . ?
C4 C6 P1 108.7(3) . . ?
C8 C7 P1 115.0(2) . . ?
C9 C8 N1 108.2(3) . . ?
C9 C8 C7 130.8(3) . . ?
N1 C8 C7 121.0(3) . . ?
C8 C9 C10 107.9(3) . . ?
C11 C10 C9 107.8(3) . . ?
C10 C11 N1 107.8(3) . . ?
C10 C11 C12 129.8(3) . . ?
N1 C11 C12 121.9(3) . . ?
C11 C12 C15 113.9(2) . . ?
C11 C12 C14 110.0(3) . . ?
C15 C12 C14 109.0(3) . . ?
C11 C12 C13 108.1(3) . . ?
C15 C12 C13 107.4(3) . . ?
C14 C12 C13 108.1(3) . . ?
C16 C15 N2 107.4(3) . . ?
C16 C15 C12 130.7(3) . . ?
N2 C15 C12 121.2(3) . . ?
C15 C16 C17 108.3(3) . . ?
C18 C17 C16 107.2(3) . . ?
C17 C18 N2 108.5(3) . . ?
C17 C18 C19 130.0(3) . . ?
N2 C18 C19 121.5(3) . . ?
C18 C19 P2 114.8(2) . . ?
C21 C20 C22 110.7(4) . . ?
C21 C20 P2 110.1(3) . . ?
C22 C20 P2 112.7(4) . . ?
C24 C23 C25 113.8(5) . . ?
C24 C23 P2 109.4(4) . . ?
C25 C23 P2 112.5(4) . . ?
N2 Ge1 N1 97.16(11) . . ?
N2 Ge1 Cl1 102.57(8) . . ?
N1 Ge1 Cl1 104.88(9) . . ?
N2 Ge1 Pd1 118.18(8) . . ?
N1 Ge1 Pd1 118.56(8) . . ?
Cl1 Ge1 Pd1 113.07(3) . . ?
C11 N1 C8 108.3(3) . . ?
C11 N1 Ge1 125.7(2) . . ?
C8 N1 Ge1 122.9(2) . . ?
C18 N2 C15 108.6(3) . . ?
C18 N2 Ge1 123.0(2) . . ?
C15 N2 Ge1 127.2(2) . . ?
C6 P1 C3 108.7(2) . . ?
C6 P1 C7 108.1(2) . . ?
C3 P1 C7 104.61(17) . . ?
C6 P1 Pd1 107.37(14) . . ?
C3 P1 Pd1 109.52(18) . . ?
C7 P1 Pd1 118.26(11) . . ?
C23 P2 C20 108.7(2) . . ?
C23 P2 C19 103.08(17) . . ?
C20 P2 C19 103.46(18) . . ?
C23 P2 Pd1 109.56(17) . . ?
C20 P2 Pd1 114.41(13) . . ?
C19 P2 Pd1 116.76(12) . . ?
Ge1 Pd1 P1 88.85(2) . . ?
Ge1 Pd1 P2 88.89(2) . . ?
P1 Pd1 P2 177.51(3) . . ?
Ge1 Pd1 Cl2 178.00(3) . . ?
P1 Pd1 Cl2 89.15(3) . . ?
P2 Pd1 Cl2 93.12(3) . . ?

_refine_diff_density_max         1.080
_refine_diff_density_min         -0.849
_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_4
_database_code_depnum_ccdc_archive 'CCDC 2035175'
loop_
_audit_author_name
_audit_author_address
'Javier A. Cabeza'
;Universidad de Oviedo
Spain
;
_audit_update_record             
;
2020-10-02 deposited with the CCDC.	2020-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H52 Ge N2 P2 Pd S2'
_chemical_formula_sum            'C37 H52 Ge N2 P2 Pd S2'
_chemical_formula_weight         829.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
Ge Ge -1.0885 0.8855 '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'
S S 0.3331 0.5567 '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                   17.5001(4)
_cell_length_b                   12.1142(2)
_cell_length_c                   18.9450(4)
_cell_angle_alpha                90
_cell_angle_beta                 114.6700(10)
_cell_angle_gamma                90
_cell_volume                     3649.75(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9882
_cell_measurement_theta_min      2.8905
_cell_measurement_theta_max      74.6585

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_F_000             1712
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    7.101
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4706
_exptl_absorpt_correction_T_max  0.6308
_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      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON III-14'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            176781
_diffrn_reflns_av_unetI/netI     0.0115
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.890
_diffrn_reflns_theta_max         74.487
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7461
_reflns_number_gt                7173
_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-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    
'MERCURY (Cambridge Crystallographic Data Centre: Cambridge, UK, 2020)'

_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)+(0.0156P)²+3.1910P] 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         7461
_refine_ls_number_parameters     416
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0190
_refine_ls_R_factor_gt           0.0178
_refine_ls_wR_factor_ref         0.0418
_refine_ls_wR_factor_gt          0.0410
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.88562(11) 0.28198(14) 0.47118(10) 0.0217(4) Uani 1 1 d . . . . .
H1A H 0.8638 0.3427 0.4339 0.033 Uiso 1 1 calc R U . . .
H1B H 0.8424 0.2583 0.4881 0.033 Uiso 1 1 calc R U . . .
H1C H 0.9009 0.2199 0.4465 0.033 Uiso 1 1 calc R U . . .
C2 C 1.03370(11) 0.35347(14) 0.51724(11) 0.0212(4) Uani 1 1 d . . . . .
H2A H 1.0501 0.2888 0.4957 0.032 Uiso 1 1 calc R U . . .
H2B H 1.0824 0.3805 0.5626 0.032 Uiso 1 1 calc R U . . .
H2C H 1.0134 0.4117 0.4778 0.032 Uiso 1 1 calc R U . . .
C3 C 0.96353(10) 0.32115(13) 0.54170(9) 0.0151(3) Uani 1 1 d . . . . .
H3 H 0.9473 0.3891 0.5621 0.018 Uiso 1 1 calc R U . . .
C4 C 1.12841(10) 0.19511(15) 0.76839(9) 0.0196(3) Uani 1 1 d . . . . .
H4A H 1.1831 0.2223 0.8058 0.029 Uiso 1 1 calc R U . . .
H4B H 1.1342 0.1186 0.7545 0.029 Uiso 1 1 calc R U . . .
H4C H 1.0879 0.1984 0.7917 0.029 Uiso 1 1 calc R U . . .
C5 C 1.09109(10) 0.38816(14) 0.71652(11) 0.0208(3) Uani 1 1 d . . . . .
H5A H 1.0476 0.3952 0.7361 0.031 Uiso 1 1 calc R U . . .
H5B H 1.0764 0.4345 0.6703 0.031 Uiso 1 1 calc R U . . .
H5C H 1.1453 0.4120 0.7567 0.031 Uiso 1 1 calc R U . . .
C6 C 1.09727(10) 0.26706(13) 0.69527(9) 0.0154(3) Uani 1 1 d . . . . .
H6 H 1.1402 0.2630 0.6733 0.019 Uiso 1 1 calc R U . . .
C7 C 1.02784(10) 0.10050(12) 0.57404(9) 0.0134(3) Uani 1 1 d . . . . .
H7A H 0.9767 0.0679 0.5330 0.016 Uiso 1 1 calc R U . . .
H7B H 1.0628 0.1301 0.5487 0.016 Uiso 1 1 calc R U . . .
C8 C 1.07564(10) 0.01143(12) 0.62892(9) 0.0127(3) Uani 1 1 d . . . . .
C9 C 1.15855(10) -0.01783(13) 0.65531(10) 0.0164(3) Uani 1 1 d . . . . .
H9 H 1.1987 0.0133 0.6395 0.020 Uiso 1 1 calc R U . . .
C10 C 1.17338(10) -0.10344(13) 0.71084(10) 0.0162(3) Uani 1 1 d . . . . .
H10 H 1.2254 -0.1400 0.7388 0.019 Uiso 1 1 calc R U . . .
C11 C 1.09916(9) -0.12380(12) 0.71690(9) 0.0123(3) Uani 1 1 d . . . . .
C12 C 1.07634(9) -0.21276(12) 0.76070(9) 0.0129(3) Uani 1 1 d . . . . .
C13 C 1.02850(10) -0.30602(13) 0.70346(9) 0.0161(3) Uani 1 1 d . . . . .
H13A H 0.9765 -0.2764 0.6632 0.024 Uiso 1 1 calc R U . . .
H13B H 1.0149 -0.3650 0.7317 0.024 Uiso 1 1 calc R U . . .
H13C H 1.0639 -0.3357 0.6792 0.024 Uiso 1 1 calc R U . . .
C14 C 1.15645(10) -0.26318(14) 0.82348(9) 0.0182(3) Uani 1 1 d . . . . .
H14A H 1.1907 -0.2955 0.7990 0.027 Uiso 1 1 calc R U . . .
H14B H 1.1410 -0.3207 0.8515 0.027 Uiso 1 1 calc R U . . .
H14C H 1.1887 -0.2054 0.8600 0.027 Uiso 1 1 calc R U . . .
C15 C 1.02045(9) -0.16716(12) 0.79695(9) 0.0118(3) Uani 1 1 d . . . . .
C16 C 1.02107(10) -0.18650(13) 0.86839(9) 0.0147(3) Uani 1 1 d . . . . .
H16 H 1.0624 -0.2271 0.9095 0.018 Uiso 1 1 calc R U . . .
C17 C 0.94876(10) -0.13506(13) 0.87014(9) 0.0146(3) Uani 1 1 d . . . . .
H17 H 0.9330 -0.1350 0.9125 0.017 Uiso 1 1 calc R U . . .
C18 C 0.90615(9) -0.08571(12) 0.79951(9) 0.0120(3) Uani 1 1 d . . . . .
C19 C 0.82330(9) -0.02661(12) 0.76685(9) 0.0121(3) Uani 1 1 d . . . . .
H19A H 0.7962 -0.0360 0.8031 0.015 Uiso 1 1 calc R U . . .
H19B H 0.7865 -0.0618 0.7170 0.015 Uiso 1 1 calc R U . . .
C20 C 0.88300(10) 0.18498(13) 0.84806(9) 0.0143(3) Uani 1 1 d . . . . .
H20 H 0.8583 0.2601 0.8453 0.017 Uiso 1 1 calc R U . . .
C21 C 0.97709(10) 0.20000(15) 0.87099(10) 0.0207(3) Uani 1 1 d . . . . .
H21A H 1.0037 0.2314 0.9234 0.031 Uiso 1 1 calc R U . . .
H21B H 0.9854 0.2500 0.8341 0.031 Uiso 1 1 calc R U . . .
H21C H 1.0026 0.1282 0.8702 0.031 Uiso 1 1 calc R U . . .
C22 C 0.87043(10) 0.12120(13) 0.91238(9) 0.0171(3) Uani 1 1 d . . . . .
H22A H 0.8999 0.0503 0.9209 0.026 Uiso 1 1 calc R U . . .
H22B H 0.8103 0.1082 0.8968 0.026 Uiso 1 1 calc R U . . .
H22C H 0.8931 0.1644 0.9605 0.026 Uiso 1 1 calc R U . . .
C23 C 0.72059(9) 0.17069(12) 0.71055(9) 0.0124(3) Uani 1 1 d . . . . .
H23 H 0.7208 0.2499 0.6958 0.015 Uiso 1 1 calc R U . . .
C24 C 0.66711(10) 0.10742(14) 0.63623(9) 0.0168(3) Uani 1 1 d . . . . .
H24A H 0.6565 0.0326 0.6497 0.025 Uiso 1 1 calc R U . . .
H24B H 0.6971 0.1034 0.6027 0.025 Uiso 1 1 calc R U . . .
H24C H 0.6135 0.1458 0.6087 0.025 Uiso 1 1 calc R U . . .
C25 C 0.67868(10) 0.16528(13) 0.76711(9) 0.0162(3) Uani 1 1 d . . . . .
H25A H 0.6200 0.1891 0.7405 0.024 Uiso 1 1 calc R U . . .
H25B H 0.7086 0.2140 0.8114 0.024 Uiso 1 1 calc R U . . .
H25C H 0.6807 0.0893 0.7856 0.024 Uiso 1 1 calc R U . . .
C26 C 0.75153(9) -0.06014(13) 0.51964(8) 0.0126(3) Uani 1 1 d . . . . .
C27 C 0.68397(10) -0.11435(13) 0.52506(10) 0.0181(3) Uani 1 1 d . . . . .
H27 H 0.6933 -0.1797 0.5553 0.022 Uiso 1 1 calc R U . . .
C28 C 0.60291(11) -0.07305(15) 0.48637(11) 0.0262(4) Uani 1 1 d . . . . .
H28 H 0.5571 -0.1100 0.4905 0.031 Uiso 1 1 calc R U . . .
C29 C 0.58875(11) 0.02152(17) 0.44197(11) 0.0294(4) Uani 1 1 d . . . . .
H29 H 0.5332 0.0487 0.4147 0.035 Uiso 1 1 calc R U . . .
C30 C 0.65573(12) 0.07637(15) 0.43740(10) 0.0273(4) Uani 1 1 d . . . . .
H30 H 0.6460 0.1420 0.4074 0.033 Uiso 1 1 calc R U . . .
C31 C 0.73723(11) 0.03647(14) 0.47621(9) 0.0191(3) Uani 1 1 d . . . . .
H31 H 0.7830 0.0750 0.4731 0.023 Uiso 1 1 calc R U . . .
C32 C 0.81230(9) 0.40928(12) 0.60245(9) 0.0129(3) Uani 1 1 d . . . . .
C33 C 0.74202(10) 0.35116(14) 0.55139(10) 0.0181(3) Uani 1 1 d . . . . .
H33 H 0.7282 0.2820 0.5667 0.022 Uiso 1 1 calc R U . . .
C34 C 0.69218(11) 0.39368(15) 0.47843(10) 0.0230(4) Uani 1 1 d . . . . .
H34 H 0.6451 0.3526 0.4440 0.028 Uiso 1 1 calc R U . . .
C35 C 0.71010(11) 0.49525(15) 0.45509(10) 0.0221(4) Uani 1 1 d . . . . .
H35 H 0.6756 0.5239 0.4052 0.027 Uiso 1 1 calc R U . . .
C36 C 0.77915(11) 0.55433(14) 0.50571(10) 0.0188(3) Uani 1 1 d . . . . .
H36 H 0.7917 0.6244 0.4906 0.023 Uiso 1 1 calc R U . . .
C37 C 0.83018(10) 0.51183(13) 0.57839(9) 0.0150(3) Uani 1 1 d . . . . .
H37 H 0.8777 0.5527 0.6122 0.018 Uiso 1 1 calc R U . . .
Ge1 Ge 0.93261(2) -0.01924(2) 0.66515(2) 0.00892(4) Uani 1 1 d . . . . .
N1 N 1.03827(8) -0.05333(10) 0.66615(7) 0.0114(2) Uani 1 1 d . . . . .
N2 N 0.94967(8) -0.10454(10) 0.75382(7) 0.0110(2) Uani 1 1 d . . . . .
P1 P 0.99614(2) 0.21623(3) 0.61970(2) 0.01063(7) Uani 1 1 d . . . . .
P2 P 0.83044(2) 0.12210(3) 0.74997(2) 0.00975(7) Uani 1 1 d . . . . .
Pd1 Pd 0.90287(2) 0.16935(2) 0.67508(2) 0.00859(3) Uani 1 1 d . . . . .
S1 S 0.85243(2) -0.12333(3) 0.56101(2) 0.01662(8) Uani 1 1 d . . . . .
S2 S 0.87647(2) 0.35817(3) 0.69626(2) 0.01283(7) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C3 1.532(2) . ?
C2 C3 1.533(2) . ?
C3 P1 1.8496(16) . ?
C4 C6 1.531(2) . ?
C5 C6 1.537(2) . ?
C6 P1 1.8563(16) . ?
C7 C8 1.490(2) . ?
C7 P1 1.8500(15) . ?
C8 C9 1.369(2) . ?
C8 N1 1.3877(19) . ?
C9 C10 1.422(2) . ?
C10 C11 1.373(2) . ?
C11 N1 1.3904(19) . ?
C11 C12 1.512(2) . ?
C12 C15 1.515(2) . ?
C12 C14 1.537(2) . ?
C12 C13 1.548(2) . ?
C15 C16 1.369(2) . ?
C15 N2 1.3901(19) . ?
C16 C17 1.423(2) . ?
C17 C18 1.368(2) . ?
C18 N2 1.3897(19) . ?
C18 C19 1.500(2) . ?
C19 P2 1.8429(15) . ?
C20 C21 1.528(2) . ?
C20 C22 1.534(2) . ?
C20 P2 1.8581(16) . ?
C23 C24 1.532(2) . ?
C23 C25 1.532(2) . ?
C23 P2 1.8442(15) . ?
C26 C31 1.392(2) . ?
C26 C27 1.393(2) . ?
C26 S1 1.7785(15) . ?
C27 C28 1.390(2) . ?
C28 C29 1.381(3) . ?
C29 C30 1.381(3) . ?
C30 C31 1.390(2) . ?
C32 C33 1.397(2) . ?
C32 C37 1.403(2) . ?
C32 S2 1.7710(16) . ?
C33 C34 1.389(2) . ?
C34 C35 1.387(3) . ?
C35 C36 1.387(2) . ?
C36 C37 1.390(2) . ?
Ge1 N2 1.8869(12) . ?
Ge1 N1 1.8870(12) . ?
Ge1 S1 2.2673(4) . ?
Ge1 Pd1 2.36801(19) . ?
P1 Pd1 2.3488(4) . ?
P2 Pd1 2.3343(4) . ?
Pd1 S2 2.4003(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
C1 C3 C2 110.43(14) . . ?
C1 C3 P1 110.45(11) . . ?
C2 C3 P1 113.45(11) . . ?
C4 C6 C5 110.11(13) . . ?
C4 C6 P1 111.93(11) . . ?
C5 C6 P1 111.71(11) . . ?
C8 C7 P1 114.40(11) . . ?
C9 C8 N1 108.69(13) . . ?
C9 C8 C7 130.02(14) . . ?
N1 C8 C7 121.18(13) . . ?
C8 C9 C10 107.29(14) . . ?
C11 C10 C9 107.82(14) . . ?
C10 C11 N1 108.08(13) . . ?
C10 C11 C12 130.51(14) . . ?
N1 C11 C12 121.03(13) . . ?
C11 C12 C15 110.94(12) . . ?
C11 C12 C14 110.09(13) . . ?
C15 C12 C14 110.32(12) . . ?
C11 C12 C13 108.98(12) . . ?
C15 C12 C13 108.73(12) . . ?
C14 C12 C13 107.70(13) . . ?
C16 C15 N2 108.17(13) . . ?
C16 C15 C12 130.21(14) . . ?
N2 C15 C12 121.20(13) . . ?
C15 C16 C17 107.93(13) . . ?
C18 C17 C16 107.19(13) . . ?
C17 C18 N2 108.71(13) . . ?
C17 C18 C19 130.59(14) . . ?
N2 C18 C19 120.55(13) . . ?
C18 C19 P2 114.48(10) . . ?
C21 C20 C22 109.19(13) . . ?
C21 C20 P2 110.98(11) . . ?
C22 C20 P2 114.37(11) . . ?
C24 C23 C25 109.53(13) . . ?
C24 C23 P2 110.26(10) . . ?
C25 C23 P2 115.18(11) . . ?
C31 C26 C27 119.42(15) . . ?
C31 C26 S1 121.53(12) . . ?
C27 C26 S1 118.79(12) . . ?
C28 C27 C26 120.15(16) . . ?
C29 C28 C27 120.26(17) . . ?
C28 C29 C30 119.74(16) . . ?
C29 C30 C31 120.63(17) . . ?
C30 C31 C26 119.78(16) . . ?
C33 C32 C37 118.20(14) . . ?
C33 C32 S2 121.67(12) . . ?
C37 C32 S2 120.11(12) . . ?
C34 C33 C32 120.52(15) . . ?
C35 C34 C33 120.97(16) . . ?
C34 C35 C36 119.01(16) . . ?
C35 C36 C37 120.51(15) . . ?
C36 C37 C32 120.78(15) . . ?
N2 Ge1 N1 94.64(5) . . ?
N2 Ge1 S1 106.30(4) . . ?
N1 Ge1 S1 97.76(4) . . ?
N2 Ge1 Pd1 114.58(4) . . ?
N1 Ge1 Pd1 117.21(4) . . ?
S1 Ge1 Pd1 121.936(12) . . ?
C8 N1 C11 108.11(12) . . ?
C8 N1 Ge1 122.61(10) . . ?
C11 N1 Ge1 127.31(10) . . ?
C18 N2 C15 108.00(12) . . ?
C18 N2 Ge1 122.71(10) . . ?
C15 N2 Ge1 126.38(10) . . ?
C3 P1 C7 101.53(7) . . ?
C3 P1 C6 105.38(7) . . ?
C7 P1 C6 103.69(7) . . ?
C3 P1 Pd1 118.87(5) . . ?
C7 P1 Pd1 115.19(5) . . ?
C6 P1 Pd1 110.63(5) . . ?
C19 P2 C23 104.34(7) . . ?
C19 P2 C20 105.56(7) . . ?
C23 P2 C20 105.75(7) . . ?
C19 P2 Pd1 116.01(5) . . ?
C23 P2 Pd1 114.47(5) . . ?
C20 P2 Pd1 109.85(5) . . ?
P2 Pd1 P1 170.293(14) . . ?
P2 Pd1 Ge1 90.275(10) . . ?
P1 Pd1 Ge1 88.915(10) . . ?
P2 Pd1 S2 86.606(13) . . ?
P1 Pd1 S2 93.578(13) . . ?
Ge1 Pd1 S2 175.348(10) . . ?
C26 S1 Ge1 106.50(5) . . ?
C32 S2 Pd1 104.54(5) . . ?

_refine_diff_density_max         0.422
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.051

_shelxl_version_number           2014-3

