# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1516699'
_audit_update_record             
;
2016-11-11 deposited with the CCDC.
2016-12-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H44 Cl Ge N2 O P2 Rh'
_chemical_formula_sum            'C25 H44 Cl Ge N2 O P2 Rh'
_chemical_formula_weight         661.51

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Rh Rh 0.0927 3.6045 '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'

_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                   9.97090(10)
_cell_length_b                   20.7798(3)
_cell_length_c                   14.2744(2)
_cell_angle_alpha                90
_cell_angle_beta                 98.8720(10)
_cell_angle_gamma                90
_cell_volume                     2922.17(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    152(2)
_cell_measurement_reflns_used    8442
_cell_measurement_theta_min      3.7790
_cell_measurement_theta_max      69.6260

_exptl_crystal_description       fragment
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_F_000             1360
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    7.859
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.58592
_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      152(2)
_diffrn_radiation_wavelength     1.54184
_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            14287
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.788
_diffrn_reflns_theta_max         69.671
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5396
_reflns_number_gt                4857
_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, 2016)'
_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)+(0.0339P)²+1.0970P] 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         5396
_refine_ls_number_parameters     310
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0266
_refine_ls_wR_factor_ref         0.0666
_refine_ls_wR_factor_gt          0.0639
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.51486(2) 0.64529(2) 0.22472(2) 0.02073(7) Uani 1 1 d . . . . .
Ge1 Ge 0.35494(3) 0.58567(2) 0.29475(2) 0.02068(8) Uani 1 1 d . . . . .
P2 P 0.32327(6) 0.66318(3) 0.11166(4) 0.02207(14) Uani 1 1 d . . . . .
Cl1 Cl 0.24506(6) 0.60715(3) 0.41516(4) 0.02928(14) Uani 1 1 d . . . . .
P1 P 0.66243(6) 0.57662(3) 0.32157(4) 0.02218(14) Uani 1 1 d . . . . .
O101 O 0.7194(2) 0.72673(13) 0.14311(18) 0.0557(7) Uani 1 1 d . . . . .
C18 C 0.1053(3) 0.75338(15) 0.0518(2) 0.0365(7) Uani 1 1 d . . . . .
H18A H 0.0542 0.7901 0.0709 0.055 Uiso 1 1 calc R U . . .
H18B H 0.0447 0.7162 0.0394 0.055 Uiso 1 1 calc R U . . .
H18C H 0.1424 0.7643 -0.0059 0.055 Uiso 1 1 calc R U . . .
N1 N 0.4234(2) 0.50349(10) 0.31990(15) 0.0245(4) Uani 1 1 d . . . . .
C19 C 0.1612(3) 0.72466(14) 0.2225(2) 0.0326(6) Uani 1 1 d . . . . .
H19A H 0.1091 0.7624 0.2368 0.049 Uiso 1 1 calc R U . . .
H19B H 0.2348 0.7167 0.2752 0.049 Uiso 1 1 calc R U . . .
H19C H 0.1014 0.6870 0.2136 0.049 Uiso 1 1 calc R U . . .
C101 C 0.6431(3) 0.69362(15) 0.17057(19) 0.0325(6) Uani 1 1 d . . . . .
C8 C 0.8076(3) 0.54466(14) 0.2647(2) 0.0313(6) Uani 1 1 d . . . . .
C6 C 0.8763(3) 0.48446(15) 0.3124(3) 0.0422(7) Uani 1 1 d . . . . .
H6A H 0.9511 0.4714 0.2794 0.063 Uiso 1 1 calc R U . . .
H6B H 0.8099 0.4495 0.3094 0.063 Uiso 1 1 calc R U . . .
H6C H 0.9118 0.4940 0.3788 0.063 Uiso 1 1 calc R U . . .
C7 C 0.7500(4) 0.52858(18) 0.1615(2) 0.0481(8) Uani 1 1 d . . . . .
H7A H 0.7121 0.5676 0.1291 0.072 Uiso 1 1 calc R U . . .
H7B H 0.6785 0.4961 0.1601 0.072 Uiso 1 1 calc R U . . .
H7C H 0.8227 0.5118 0.1294 0.072 Uiso 1 1 calc R U . . .
C5 C 0.9150(3) 0.59719(16) 0.2638(2) 0.0402(7) Uani 1 1 d . . . . .
H5A H 0.9854 0.5820 0.2282 0.060 Uiso 1 1 calc R U . . .
H5B H 0.9560 0.6072 0.3290 0.060 Uiso 1 1 calc R U . . .
H5C H 0.8723 0.6360 0.2335 0.060 Uiso 1 1 calc R U . . .
N2 N 0.2234(2) 0.55462(10) 0.19835(14) 0.0232(4) Uani 1 1 d . . . . .
C20 C 0.2216(3) 0.73698(13) 0.13128(19) 0.0272(5) Uani 1 1 d . . . . .
C16 C 0.2008(3) 0.59317(12) 0.11186(18) 0.0249(5) Uani 1 1 d . . . . .
H16A H 0.1070 0.6102 0.1031 0.030 Uiso 1 1 calc R U . . .
H16B H 0.2090 0.5650 0.0571 0.030 Uiso 1 1 calc R U . . .
C17 C 0.3188(3) 0.79425(13) 0.1492(2) 0.0330(6) Uani 1 1 d . . . . .
H17A H 0.3576 0.8035 0.0915 0.049 Uiso 1 1 calc R U . . .
H17B H 0.3920 0.7839 0.2010 0.049 Uiso 1 1 calc R U . . .
H17C H 0.2691 0.8321 0.1663 0.049 Uiso 1 1 calc R U . . .
C10 C 0.3500(3) 0.46058(13) 0.25539(18) 0.0258(5) Uani 1 1 d . . . . .
C14 C 0.1639(3) 0.44842(14) 0.1246(2) 0.0333(6) Uani 1 1 d . . . . .
H14 H 0.0913 0.4662 0.0816 0.040 Uiso 1 1 calc R U . . .
C9 C 0.5710(3) 0.49862(13) 0.3413(2) 0.0310(6) Uani 1 1 d . . . . .
H9A H 0.6020 0.4646 0.3011 0.037 Uiso 1 1 calc R U . . .
H9B H 0.5966 0.4853 0.4083 0.037 Uiso 1 1 calc R U . . .
C3 C 0.8387(3) 0.57206(17) 0.5038(2) 0.0437(8) Uani 1 1 d . . . . .
H3A H 0.9224 0.5749 0.4759 0.066 Uiso 1 1 calc R U . . .
H3B H 0.8113 0.5269 0.5063 0.066 Uiso 1 1 calc R U . . .
H3C H 0.8545 0.5899 0.5681 0.066 Uiso 1 1 calc R U . . .
C2 C 0.7724(3) 0.67974(15) 0.4310(2) 0.0385(7) Uani 1 1 d . . . . .
H2A H 0.7895 0.7008 0.4931 0.058 Uiso 1 1 calc R U . . .
H2B H 0.7014 0.7032 0.3895 0.058 Uiso 1 1 calc R U . . .
H2C H 0.8559 0.6796 0.4027 0.058 Uiso 1 1 calc R U . . .
C23 C 0.2287(3) 0.64701(15) -0.0883(2) 0.0358(7) Uani 1 1 d . . . . .
H23A H 0.1679 0.6842 -0.0896 0.054 Uiso 1 1 calc R U . . .
H23B H 0.1819 0.6083 -0.0709 0.054 Uiso 1 1 calc R U . . .
H23C H 0.2549 0.6411 -0.1512 0.054 Uiso 1 1 calc R U . . .
C1 C 0.6032(3) 0.61295(18) 0.4955(2) 0.0414(7) Uani 1 1 d . . . . .
H1A H 0.5735 0.5691 0.5070 0.062 Uiso 1 1 calc R U . . .
H1B H 0.5290 0.6363 0.4570 0.062 Uiso 1 1 calc R U . . .
H1C H 0.6286 0.6351 0.5562 0.062 Uiso 1 1 calc R U . . .
C4 C 0.7260(3) 0.61030(14) 0.44278(18) 0.0294(6) Uani 1 1 d . . . . .
C22 C 0.4546(3) 0.60185(15) -0.0187(2) 0.0362(7) Uani 1 1 d . . . . .
H22A H 0.4693 0.5952 -0.0843 0.054 Uiso 1 1 calc R U . . .
H22B H 0.4153 0.5629 0.0046 0.054 Uiso 1 1 calc R U . . .
H22C H 0.5415 0.6113 0.0211 0.054 Uiso 1 1 calc R U . . .
C21 C 0.4253(3) 0.72024(15) -0.0424(2) 0.0350(6) Uani 1 1 d . . . . .
H21A H 0.5042 0.7299 0.0055 0.053 Uiso 1 1 calc R U . . .
H21B H 0.3607 0.7560 -0.0462 0.053 Uiso 1 1 calc R U . . .
H21C H 0.4549 0.7142 -0.1041 0.053 Uiso 1 1 calc R U . . .
C11 C 0.3760(3) 0.39517(13) 0.2505(2) 0.0309(6) Uani 1 1 d . . . . .
H11 H 0.4482 0.3765 0.2930 0.037 Uiso 1 1 calc R U . . .
C24 C 0.3569(3) 0.65873(14) -0.01471(18) 0.0293(6) Uani 1 1 d . . . . .
C15 C 0.2419(3) 0.48794(13) 0.19095(18) 0.0249(5) Uani 1 1 d . . . . .
C12 C 0.2967(3) 0.35662(14) 0.1835(2) 0.0392(7) Uani 1 1 d . . . . .
H12 H 0.3150 0.3118 0.1807 0.047 Uiso 1 1 calc R U . . .
C13 C 0.1924(3) 0.38319(15) 0.1215(2) 0.0422(7) Uani 1 1 d . . . . .
H13 H 0.1391 0.3566 0.0760 0.051 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 C101 1.883(3) . ?
Rh1 P2 2.3327(6) . ?
Rh1 P1 2.3420(6) . ?
Rh1 Ge1 2.3596(3) . ?
Ge1 N1 1.853(2) . ?
Ge1 N2 1.864(2) . ?
Ge1 Cl1 2.2213(7) . ?
P2 C20 1.883(3) . ?
P2 C24 1.887(3) . ?
P2 C16 1.899(3) . ?
P1 C4 1.883(3) . ?
P1 C8 1.886(3) . ?
P1 C9 1.902(3) . ?
O101 C101 1.139(4) . ?
C18 C20 1.531(4) . ?
N1 C10 1.404(3) . ?
N1 C9 1.460(3) . ?
C19 C20 1.538(4) . ?
C8 C5 1.531(4) . ?
C8 C6 1.534(4) . ?
C8 C7 1.534(4) . ?
N2 C15 1.404(3) . ?
N2 C16 1.460(3) . ?
C20 C17 1.531(4) . ?
C10 C11 1.388(4) . ?
C10 C15 1.423(4) . ?
C14 C13 1.387(4) . ?
C14 C15 1.396(4) . ?
C3 C4 1.533(4) . ?
C2 C4 1.532(4) . ?
C23 C24 1.544(4) . ?
C1 C4 1.534(4) . ?
C22 C24 1.538(4) . ?
C21 C24 1.529(4) . ?
C11 C12 1.396(4) . ?
C12 C13 1.373(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C101 Rh1 P2 99.58(8) . . ?
C101 Rh1 P1 99.37(8) . . ?
P2 Rh1 P1 151.46(2) . . ?
C101 Rh1 Ge1 179.11(9) . . ?
P2 Rh1 Ge1 80.905(18) . . ?
P1 Rh1 Ge1 80.458(18) . . ?
N1 Ge1 N2 91.15(9) . . ?
N1 Ge1 Cl1 104.24(7) . . ?
N2 Ge1 Cl1 105.42(7) . . ?
N1 Ge1 Rh1 108.25(7) . . ?
N2 Ge1 Rh1 108.28(7) . . ?
Cl1 Ge1 Rh1 131.95(2) . . ?
C20 P2 C24 111.17(12) . . ?
C20 P2 C16 105.23(12) . . ?
C24 P2 C16 99.95(12) . . ?
C20 P2 Rh1 115.41(8) . . ?
C24 P2 Rh1 113.97(9) . . ?
C16 P2 Rh1 109.56(8) . . ?
C4 P1 C8 110.73(12) . . ?
C4 P1 C9 106.36(13) . . ?
C8 P1 C9 100.43(13) . . ?
C4 P1 Rh1 114.06(9) . . ?
C8 P1 Rh1 114.51(9) . . ?
C9 P1 Rh1 109.56(8) . . ?
C10 N1 C9 120.0(2) . . ?
C10 N1 Ge1 108.61(16) . . ?
C9 N1 Ge1 115.69(16) . . ?
O101 C101 Rh1 174.3(3) . . ?
C5 C8 C6 108.7(2) . . ?
C5 C8 C7 107.8(3) . . ?
C6 C8 C7 108.9(3) . . ?
C5 C8 P1 109.7(2) . . ?
C6 C8 P1 114.6(2) . . ?
C7 C8 P1 106.96(19) . . ?
C15 N2 C16 118.9(2) . . ?
C15 N2 Ge1 108.16(16) . . ?
C16 N2 Ge1 115.68(16) . . ?
C18 C20 C17 109.8(2) . . ?
C18 C20 C19 108.3(2) . . ?
C17 C20 C19 108.0(2) . . ?
C18 C20 P2 115.8(2) . . ?
C17 C20 P2 108.45(18) . . ?
C19 C20 P2 106.29(18) . . ?
N2 C16 P2 113.98(16) . . ?
C11 C10 N1 124.9(2) . . ?
C11 C10 C15 119.2(2) . . ?
N1 C10 C15 115.9(2) . . ?
C13 C14 C15 120.1(3) . . ?
N1 C9 P1 113.62(18) . . ?
C2 C4 C3 110.1(2) . . ?
C2 C4 C1 107.3(3) . . ?
C3 C4 C1 108.1(2) . . ?
C2 C4 P1 108.26(18) . . ?
C3 C4 P1 116.3(2) . . ?
C1 C4 P1 106.42(19) . . ?
C10 C11 C12 120.4(3) . . ?
C21 C24 C22 108.8(2) . . ?
C21 C24 C23 108.2(2) . . ?
C22 C24 C23 108.4(2) . . ?
C21 C24 P2 110.97(19) . . ?
C22 C24 P2 106.25(18) . . ?
C23 C24 P2 114.1(2) . . ?
C14 C15 N2 124.5(2) . . ?
C14 C15 C10 119.4(3) . . ?
N2 C15 C10 116.2(2) . . ?
C13 C12 C11 120.2(3) . . ?
C12 C13 C14 120.7(3) . . ?

_refine_diff_density_max         1.099
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.073

_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_3
_database_code_depnum_ccdc_archive 'CCDC 1516698'
_audit_update_record             
;
2016-11-11 deposited with the CCDC.
2016-12-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H56 Cl Ge N2 P2 Rh'
_chemical_formula_sum            'C32 H56 Cl Ge N2 P2 Rh'
_chemical_formula_weight         741.67

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'
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'
Rh Rh 0.0927 3.6045 '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                   14.5188(2)
_cell_length_b                   17.9914(2)
_cell_length_c                   13.3164(2)
_cell_angle_alpha                90
_cell_angle_beta                 92.9220(10)
_cell_angle_gamma                90
_cell_volume                     3473.90(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    151(2)
_cell_measurement_reflns_used    9896
_cell_measurement_theta_min      3.8960
_cell_measurement_theta_max      69.2160

_exptl_crystal_description       fragment
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_F_000             1544
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    6.650
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.86745
_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      151(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            18304
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.048
_diffrn_reflns_theta_max         69.619
_diffrn_reflns_theta_full        90.000
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.809
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.809
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.809
_reflns_number_total             6419
_reflns_number_gt                5805
_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, 2016)'
_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)+(0.0386P)²+3.2241P] 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         6419
_refine_ls_number_parameters     364
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0306
_refine_ls_wR_factor_ref         0.0791
_refine_ls_wR_factor_gt          0.0760
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_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
Rh1 Rh 0.19286(2) 0.02209(2) 0.28997(2) 0.02525(7) Uani 1 1 d . . . . .
Ge1 Ge 0.19770(2) -0.03592(2) 0.12683(2) 0.02518(9) Uani 1 1 d . . . . .
P2 P 0.37546(5) -0.15545(4) 0.15286(5) 0.02836(15) Uani 1 1 d . . . . .
P1 P 0.12852(5) 0.12157(4) 0.19229(5) 0.02554(15) Uani 1 1 d . . . . .
Cl1 Cl 0.10230(5) -0.13745(4) 0.11479(5) 0.03864(17) Uani 1 1 d . . . . .
C28 C 0.3115(2) 0.06632(19) 0.4745(2) 0.0416(7) Uani 1 1 d . . . . .
H28A H 0.3157 0.0808 0.5463 0.050 Uiso 1 1 calc R U . . .
H28B H 0.3585 0.0951 0.4397 0.050 Uiso 1 1 calc R U . . .
C10 C 0.1766(2) 0.02380(15) -0.0615(2) 0.0287(6) Uani 1 1 d . . . . .
C30 C 0.1379(2) 0.04540(18) 0.4392(2) 0.0350(7) Uani 1 1 d . . . . .
H30 H 0.0804 0.0761 0.4354 0.042 Uiso 1 1 calc R U . . .
C27 C 0.3338(2) -0.01637(18) 0.4662(2) 0.0381(7) Uani 1 1 d . . . . .
H27A H 0.4015 -0.0227 0.4677 0.046 Uiso 1 1 calc R U . . .
H27B H 0.3107 -0.0425 0.5254 0.046 Uiso 1 1 calc R U . . .
N1 N 0.14613(17) 0.03135(13) 0.03441(17) 0.0298(5) Uani 1 1 d . . . . .
N2 N 0.27702(16) -0.06080(13) 0.02579(16) 0.0276(5) Uani 1 1 d . . . . .
C15 C 0.24835(19) -0.02946(15) -0.0665(2) 0.0271(6) Uani 1 1 d . . . . .
C24 C 0.4921(2) -0.10915(18) 0.1666(2) 0.0347(6) Uani 1 1 d . . . . .
C29 C 0.2172(2) 0.08674(17) 0.4302(2) 0.0359(7) Uani 1 1 d . . . . .
H29 H 0.2064 0.1414 0.4225 0.043 Uiso 1 1 calc R U . . .
C26 C 0.2917(2) -0.05220(18) 0.3709(2) 0.0348(7) Uani 1 1 d . . . . .
H26 H 0.3390 -0.0730 0.3267 0.042 Uiso 1 1 calc R U . . .
C16 C 0.3346(2) -0.12702(16) 0.0243(2) 0.0308(6) Uani 1 1 d . . . . .
H16A H 0.3884 -0.1171 -0.0164 0.037 Uiso 1 1 calc R U . . .
H16B H 0.2988 -0.1682 -0.0080 0.037 Uiso 1 1 calc R U . . .
C20 C 0.3875(2) -0.25911(17) 0.1335(2) 0.0372(7) Uani 1 1 d . . . . .
C9 C 0.0839(2) 0.08731(17) 0.0667(2) 0.0314(6) Uani 1 1 d . . . . .
H9A H 0.0213 0.0662 0.0717 0.038 Uiso 1 1 calc R U . . .
H9B H 0.0803 0.1288 0.0178 0.038 Uiso 1 1 calc R U . . .
C4 C 0.0242(2) 0.17301(18) 0.2349(2) 0.0373(7) Uani 1 1 d . . . . .
C2 C -0.0493(2) 0.1137(2) 0.2497(3) 0.0498(9) Uani 1 1 d . . . . .
H2A H -0.0977 0.1343 0.2903 0.075 Uiso 1 1 calc R U . . .
H2B H -0.0211 0.0707 0.2843 0.075 Uiso 1 1 calc R U . . .
H2C H -0.0763 0.0982 0.1841 0.075 Uiso 1 1 calc R U . . .
C8 C 0.2248(2) 0.18680(19) 0.1585(2) 0.0440(8) Uani 1 1 d . . . . .
C3 C -0.0137(3) 0.2302(2) 0.1576(3) 0.0663(13) Uani 1 1 d . . . . .
H3A H -0.0286 0.2053 0.0934 0.099 Uiso 1 1 calc R U . . .
H3B H 0.0328 0.2687 0.1481 0.099 Uiso 1 1 calc R U . . .
H3C H -0.0696 0.2531 0.1821 0.099 Uiso 1 1 calc R U . . .
C17 C 0.4484(3) -0.2929(2) 0.2196(3) 0.0499(9) Uani 1 1 d . . . . .
H17A H 0.4469 -0.3472 0.2145 0.075 Uiso 1 1 calc R U . . .
H17B H 0.4251 -0.2776 0.2842 0.075 Uiso 1 1 calc R U . . .
H17C H 0.5119 -0.2754 0.2149 0.075 Uiso 1 1 calc R U . . .
C32 C 0.1355(3) -0.0943(2) 0.4363(2) 0.0447(8) Uani 1 1 d . . . . .
H32A H 0.1491 -0.1376 0.4804 0.054 Uiso 1 1 calc R U . . .
H32B H 0.0750 -0.1030 0.4006 0.054 Uiso 1 1 calc R U . . .
C18 C 0.4249(3) -0.28388(19) 0.0332(3) 0.0497(9) Uani 1 1 d . . . . .
H18A H 0.4300 -0.3382 0.0321 0.075 Uiso 1 1 calc R U . . .
H18B H 0.4859 -0.2618 0.0257 0.075 Uiso 1 1 calc R U . . .
H18C H 0.3827 -0.2675 -0.0222 0.075 Uiso 1 1 calc R U . . .
C31 C 0.1292(2) -0.0250(2) 0.5011(2) 0.0409(8) Uani 1 1 d . . . . .
H31A H 0.0694 -0.0247 0.5335 0.049 Uiso 1 1 calc R U . . .
H31B H 0.1789 -0.0261 0.5548 0.049 Uiso 1 1 calc R U . . .
C19 C 0.2892(3) -0.2889(2) 0.1418(3) 0.0511(9) Uani 1 1 d . . . . .
H19A H 0.2486 -0.2668 0.0889 0.077 Uiso 1 1 calc R U . . .
H19B H 0.2668 -0.2759 0.2078 0.077 Uiso 1 1 calc R U . . .
H19C H 0.2893 -0.3431 0.1341 0.077 Uiso 1 1 calc R U . . .
C23 C 0.4733(2) -0.02627(18) 0.1494(3) 0.0428(8) Uani 1 1 d . . . . .
H23A H 0.5303 0.0019 0.1633 0.064 Uiso 1 1 calc R U . . .
H23B H 0.4262 -0.0095 0.1944 0.064 Uiso 1 1 calc R U . . .
H23C H 0.4513 -0.0182 0.0794 0.064 Uiso 1 1 calc R U . . .
C12 C 0.1853(2) 0.04724(18) -0.2385(2) 0.0376(7) Uani 1 1 d . . . . .
H12 H 0.1656 0.0741 -0.2972 0.045 Uiso 1 1 calc R U . . .
C7 C 0.3143(3) 0.1375(3) 0.1520(4) 0.0671(12) Uani 1 1 d . . . . .
H7A H 0.3672 0.1694 0.1398 0.101 Uiso 1 1 calc R U . . .
H7B H 0.3055 0.1018 0.0967 0.101 Uiso 1 1 calc R U . . .
H7C H 0.3257 0.1106 0.2154 0.101 Uiso 1 1 calc R U . . .
C11 C 0.1450(2) 0.06194(17) -0.1473(2) 0.0336(6) Uani 1 1 d . . . . .
H11 H 0.0968 0.0974 -0.1440 0.040 Uiso 1 1 calc R U . . .
C5 C 0.2476(3) 0.2430(3) 0.2387(4) 0.0800(15) Uani 1 1 d . . . . .
H5A H 0.3036 0.2700 0.2224 0.120 Uiso 1 1 calc R U . . .
H5B H 0.2580 0.2177 0.3035 0.120 Uiso 1 1 calc R U . . .
H5C H 0.1963 0.2781 0.2428 0.120 Uiso 1 1 calc R U . . .
C25 C 0.2084(2) -0.08868(17) 0.3605(2) 0.0377(7) Uani 1 1 d . . . . .
H25 H 0.2078 -0.1307 0.3113 0.045 Uiso 1 1 calc R U . . .
C21 C 0.5654(2) -0.1352(2) 0.0953(3) 0.0440(8) Uani 1 1 d . . . . .
H21A H 0.5413 -0.1301 0.0256 0.066 Uiso 1 1 calc R U . . .
H21B H 0.5805 -0.1874 0.1091 0.066 Uiso 1 1 calc R U . . .
H21C H 0.6210 -0.1048 0.1058 0.066 Uiso 1 1 calc R U . . .
C14 C 0.2838(2) -0.04527(17) -0.1589(2) 0.0324(6) Uani 1 1 d . . . . .
H14 H 0.3290 -0.0831 -0.1642 0.039 Uiso 1 1 calc R U . . .
C13 C 0.2531(2) -0.00563(18) -0.2439(2) 0.0371(7) Uani 1 1 d . . . . .
H13 H 0.2793 -0.0153 -0.3065 0.045 Uiso 1 1 calc R U . . .
C1 C 0.0433(3) 0.21312(19) 0.3356(2) 0.0452(8) Uani 1 1 d . . . . .
H1A H -0.0145 0.2336 0.3588 0.068 Uiso 1 1 calc R U . . .
H1B H 0.0873 0.2536 0.3267 0.068 Uiso 1 1 calc R U . . .
H1C H 0.0691 0.1778 0.3855 0.068 Uiso 1 1 calc R U . . .
C22 C 0.5302(2) -0.1189(2) 0.2761(2) 0.0442(8) Uani 1 1 d . . . . .
H22A H 0.5874 -0.0903 0.2864 0.066 Uiso 1 1 calc R U . . .
H22B H 0.5429 -0.1716 0.2892 0.066 Uiso 1 1 calc R U . . .
H22C H 0.4846 -0.1010 0.3222 0.066 Uiso 1 1 calc R U . . .
C6 C 0.2121(4) 0.2203(3) 0.0524(4) 0.0824(16) Uani 1 1 d . . . . .
H6A H 0.1589 0.2539 0.0496 0.124 Uiso 1 1 calc R U . . .
H6B H 0.2017 0.1803 0.0032 0.124 Uiso 1 1 calc R U . . .
H6C H 0.2677 0.2481 0.0368 0.124 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 C26 2.202(3) . ?
Rh1 C25 2.210(3) . ?
Rh1 C29 2.213(3) . ?
Rh1 C30 2.219(3) . ?
Rh1 P1 2.3757(7) . ?
Rh1 Ge1 2.4144(3) . ?
Ge1 N1 1.856(2) . ?
Ge1 N2 1.869(2) . ?
Ge1 Cl1 2.2931(8) . ?
P2 C16 1.855(3) . ?
P2 C24 1.888(3) . ?
P2 C20 1.892(3) . ?
P1 C9 1.867(3) . ?
P1 C4 1.886(3) . ?
P1 C8 1.896(3) . ?
C28 C29 1.509(4) . ?
C28 C27 1.528(5) . ?
C10 N1 1.380(4) . ?
C10 C11 1.390(4) . ?
C10 C15 1.419(4) . ?
C30 C29 1.381(5) . ?
C30 C31 1.519(5) . ?
C27 C26 1.523(4) . ?
N1 C9 1.434(4) . ?
N2 C15 1.396(3) . ?
N2 C16 1.456(4) . ?
C15 C14 1.388(4) . ?
C24 C23 1.531(5) . ?
C24 C21 1.534(4) . ?
C24 C22 1.543(4) . ?
C26 C25 1.376(5) . ?
C20 C18 1.534(5) . ?
C20 C19 1.534(5) . ?
C20 C17 1.536(4) . ?
C4 C2 1.529(5) . ?
C4 C1 1.536(4) . ?
C4 C3 1.538(5) . ?
C8 C5 1.495(5) . ?
C8 C6 1.539(5) . ?
C8 C7 1.580(6) . ?
C32 C25 1.504(5) . ?
C32 C31 1.521(5) . ?
C12 C13 1.373(5) . ?
C12 C11 1.400(4) . ?
C14 C13 1.392(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
C26 Rh1 C25 36.34(12) . . ?
C26 Rh1 C29 80.45(11) . . ?
C25 Rh1 C29 96.15(11) . . ?
C26 Rh1 C30 86.07(11) . . ?
C25 Rh1 C30 79.85(12) . . ?
C29 Rh1 C30 36.30(12) . . ?
C26 Rh1 P1 162.46(9) . . ?
C25 Rh1 P1 160.22(9) . . ?
C29 Rh1 P1 96.16(8) . . ?
C30 Rh1 P1 101.46(8) . . ?
C26 Rh1 Ge1 97.47(8) . . ?
C25 Rh1 Ge1 89.16(8) . . ?
C29 Rh1 Ge1 167.36(9) . . ?
C30 Rh1 Ge1 156.33(9) . . ?
P1 Rh1 Ge1 82.047(18) . . ?
N1 Ge1 N2 85.49(10) . . ?
N1 Ge1 Cl1 104.55(8) . . ?
N2 Ge1 Cl1 98.68(8) . . ?
N1 Ge1 Rh1 106.59(7) . . ?
N2 Ge1 Rh1 142.98(7) . . ?
Cl1 Ge1 Rh1 111.23(2) . . ?
C16 P2 C24 102.19(14) . . ?
C16 P2 C20 100.00(13) . . ?
C24 P2 C20 111.08(14) . . ?
C9 P1 C4 100.61(13) . . ?
C9 P1 C8 102.62(14) . . ?
C4 P1 C8 112.33(16) . . ?
C9 P1 Rh1 110.52(10) . . ?
C4 P1 Rh1 120.28(10) . . ?
C8 P1 Rh1 108.79(11) . . ?
C29 C28 C27 113.6(3) . . ?
N1 C10 C11 127.2(3) . . ?
N1 C10 C15 112.4(2) . . ?
C11 C10 C15 120.5(3) . . ?
C29 C30 C31 126.1(3) . . ?
C29 C30 Rh1 71.61(16) . . ?
C31 C30 Rh1 111.8(2) . . ?
C26 C27 C28 113.3(2) . . ?
C10 N1 C9 125.7(2) . . ?
C10 N1 Ge1 114.33(19) . . ?
C9 N1 Ge1 119.86(18) . . ?
C15 N2 C16 117.7(2) . . ?
C15 N2 Ge1 111.70(18) . . ?
C16 N2 Ge1 125.51(18) . . ?
C14 C15 N2 126.2(3) . . ?
C14 C15 C10 119.1(3) . . ?
N2 C15 C10 114.7(2) . . ?
C23 C24 C21 109.2(3) . . ?
C23 C24 C22 107.7(3) . . ?
C21 C24 C22 108.9(3) . . ?
C23 C24 P2 105.2(2) . . ?
C21 C24 P2 116.9(2) . . ?
C22 C24 P2 108.6(2) . . ?
C30 C29 C28 125.4(3) . . ?
C30 C29 Rh1 72.10(16) . . ?
C28 C29 Rh1 107.7(2) . . ?
C25 C26 C27 126.8(3) . . ?
C25 C26 Rh1 72.13(17) . . ?
C27 C26 Rh1 112.0(2) . . ?
N2 C16 P2 111.71(18) . . ?
C18 C20 C19 109.5(3) . . ?
C18 C20 C17 108.6(3) . . ?
C19 C20 C17 108.1(3) . . ?
C18 C20 P2 116.4(2) . . ?
C19 C20 P2 104.0(2) . . ?
C17 C20 P2 110.0(2) . . ?
N1 C9 P1 107.78(18) . . ?
C2 C4 C1 108.1(3) . . ?
C2 C4 C3 108.9(3) . . ?
C1 C4 C3 108.2(3) . . ?
C2 C4 P1 105.9(2) . . ?
C1 C4 P1 112.4(2) . . ?
C3 C4 P1 113.1(2) . . ?
C5 C8 C6 113.8(4) . . ?
C5 C8 C7 105.4(3) . . ?
C6 C8 C7 103.2(4) . . ?
C5 C8 P1 112.9(3) . . ?
C6 C8 P1 113.9(3) . . ?
C7 C8 P1 106.5(2) . . ?
C25 C32 C31 113.0(3) . . ?
C30 C31 C32 111.5(2) . . ?
C13 C12 C11 120.6(3) . . ?
C10 C11 C12 119.0(3) . . ?
C26 C25 C32 127.5(3) . . ?
C26 C25 Rh1 71.52(17) . . ?
C32 C25 Rh1 106.6(2) . . ?
C15 C14 C13 119.9(3) . . ?
C12 C13 C14 120.9(3) . . ?

_refine_diff_density_max         1.478
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.071

_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_2
_database_code_depnum_ccdc_archive 'CCDC 1516697'
_audit_update_record             
;
2016-11-11 deposited with the CCDC.
2016-12-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H44 Co2 Ge N2 O6 P2'
_chemical_formula_sum            'C30 H44 Co2 Ge N2 O6 P2'
_chemical_formula_weight         781.06

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'
Co Co -2.3653 3.6143 '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'
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'
Sn Sn 0.0259 5.4591 '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                   17.2945(14)
_cell_length_b                   17.5482(8)
_cell_length_c                   22.8262(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6927.5(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    145(2)
_cell_measurement_reflns_used    4863
_cell_measurement_theta_min      3.8890
_cell_measurement_theta_max      69.0370

_exptl_crystal_description       fragment
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_F_000             3216
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    9.660
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_correction_T_min  0.0664
_exptl_absorpt_correction_T_max  0.4613
_exptl_absorpt_process_details   
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Cubic fit to sin(theta)/lambda - 24 parameters
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      145(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            10802
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.873
_diffrn_reflns_theta_max         69.709
_diffrn_reflns_theta_full        67.680
_diffrn_measured_fraction_theta_max 0.711
_diffrn_measured_fraction_theta_full 0.728
_diffrn_reflns_Laue_measured_fraction_max 0.711
_diffrn_reflns_Laue_measured_fraction_full 0.728
_diffrn_reflns_point_group_measured_fraction_max 0.711
_diffrn_reflns_point_group_measured_fraction_full 0.728
_reflns_number_total             4632
_reflns_number_gt                3180
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 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.

 Restraints were applied on the thermal parameters of the carbonyl C atoms
 of 1060_dp704f2 due to their tendency to give nonpositive definite ellipsoids.
;

_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, 2016)'
_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)+(0.1974P)²+82.3172P] 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         4632
_refine_ls_number_parameters     376
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1414
_refine_ls_R_factor_gt           0.0934
_refine_ls_wR_factor_ref         0.3534
_refine_ls_wR_factor_gt          0.2533
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_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
Ge1 Ge 0.83360(11) 0.09506(8) 0.61485(6) 0.0492(6) Uani 1 1 d . . . . .
Co1 Co 0.70245(16) 0.05826(12) 0.59236(9) 0.0507(7) Uani 1 1 d . . . . .
Co2 Co 0.87636(17) 0.07115(13) 0.71499(9) 0.0559(8) Uani 1 1 d . . . . .
P1 P 0.7493(2) 0.01160(17) 0.50715(14) 0.0457(9) Uani 1 1 d . . . . .
P2 P 0.9197(3) 0.1926(2) 0.71425(15) 0.0523(10) Uani 1 1 d . . . . .
C102 C 0.7051(10) -0.0131(9) 0.6477(6) 0.064(3) Uani 1 1 d . . . . .
O101 O 0.6799(7) 0.2194(6) 0.6172(5) 0.072(3) Uani 1 1 d . . . . .
O102 O 0.7042(8) -0.0619(7) 0.6812(5) 0.083(4) Uani 1 1 d . . . . .
N2 N 0.8747(7) 0.1928(6) 0.5992(5) 0.048(3) Uani 1 1 d . . . . .
C4 C 0.7229(9) -0.0896(7) 0.4874(7) 0.052(4) Uani 1 1 d . . . . .
C203 C 0.7853(12) 0.0719(8) 0.7470(6) 0.056(2) Uani 1 1 d . . . . .
C9 C 0.8557(9) 0.0035(7) 0.5116(6) 0.051(4) Uani 1 1 d . . . . .
H9A H 0.8698 -0.0474 0.5271 0.061 Uiso 1 1 calc R U . . .
H9B H 0.8782 0.0085 0.4719 0.061 Uiso 1 1 calc R U . . .
O202 O 0.9615(9) 0.0184(8) 0.8177(5) 0.094(4) Uani 1 1 d . . . . .
C10 C 0.9326(9) 0.1199(8) 0.5244(5) 0.053(4) Uani 1 1 d . . . . .
C17 C 0.8833(10) 0.2534(8) 0.7772(5) 0.056(4) Uani 1 1 d . . . . .
O203 O 0.7252(8) 0.0691(6) 0.7686(5) 0.065(3) Uani 1 1 d . . . . .
C3 C 0.7803(10) -0.1262(7) 0.4436(7) 0.057(4) Uani 1 1 d . . . . .
H3A H 0.8313 -0.1307 0.4620 0.086 Uiso 1 1 calc R U . . .
H3B H 0.7843 -0.0941 0.4086 0.086 Uiso 1 1 calc R U . . .
H3C H 0.7617 -0.1770 0.4324 0.086 Uiso 1 1 calc R U . . .
C101 C 0.6879(11) 0.1572(9) 0.6073(7) 0.064(3) Uani 1 1 d . . . . .
N1 N 0.8873(8) 0.0625(6) 0.5497(5) 0.056(3) Uani 1 1 d . . . . .
C8 C 0.7279(10) 0.0765(7) 0.4433(5) 0.053(4) Uani 1 1 d . . . . .
C11 C 0.9849(9) 0.1142(8) 0.4759(6) 0.054(4) Uani 1 1 d . . . . .
H11 H 0.9937 0.0661 0.4579 0.065 Uiso 1 1 calc R U . . .
C16 C 0.8831(10) 0.2448(7) 0.6487(6) 0.052(4) Uani 1 1 d . . . . .
H16A H 0.8324 0.2682 0.6579 0.063 Uiso 1 1 calc R U . . .
H16B H 0.9196 0.2861 0.6383 0.063 Uiso 1 1 calc R U . . .
C13 C 1.0169(10) 0.2471(8) 0.4840(6) 0.060(4) Uani 1 1 d . . . . .
H13 H 1.0464 0.2897 0.4712 0.072 Uiso 1 1 calc R U . . .
C201 C 0.9064(10) -0.0112(8) 0.6769(6) 0.056(2) Uani 1 1 d . . . . .
C15 C 0.9276(8) 0.1918(7) 0.5531(5) 0.040(3) Uani 1 1 d . . . . .
O201 O 0.9249(12) -0.0662(8) 0.6552(6) 0.127(7) Uani 1 1 d . . . . .
C20 C 0.9228(12) 0.3333(10) 0.7812(7) 0.079(5) Uani 1 1 d . . . . .
H20A H 0.9775 0.3270 0.7913 0.119 Uiso 1 1 calc R U . . .
H20B H 0.8971 0.3638 0.8115 0.119 Uiso 1 1 calc R U . . .
H20C H 0.9185 0.3593 0.7433 0.119 Uiso 1 1 calc R U . . .
C12 C 1.0225(9) 0.1781(8) 0.4552(6) 0.053(4) Uani 1 1 d . . . . .
H12 H 1.0526 0.1747 0.4205 0.064 Uiso 1 1 calc R U . . .
C103 C 0.6041(12) 0.0410(9) 0.5739(7) 0.064(3) Uani 1 1 d . . . . .
C7 C 0.7736(10) 0.1509(7) 0.4525(5) 0.055(4) Uani 1 1 d . . . . .
H7A H 0.8291 0.1407 0.4483 0.082 Uiso 1 1 calc R U . . .
H7B H 0.7633 0.1707 0.4919 0.082 Uiso 1 1 calc R U . . .
H7C H 0.7576 0.1886 0.4233 0.082 Uiso 1 1 calc R U . . .
C6 C 0.6424(9) 0.0974(8) 0.4411(7) 0.055(4) Uani 1 1 d . . . . .
H6A H 0.6279 0.1238 0.4773 0.083 Uiso 1 1 calc R U . . .
H6B H 0.6114 0.0509 0.4371 0.083 Uiso 1 1 calc R U . . .
H6C H 0.6328 0.1308 0.4075 0.083 Uiso 1 1 calc R U . . .
C14 C 0.9681(10) 0.2536(8) 0.5317(5) 0.061(4) Uani 1 1 d . . . . .
H14 H 0.9623 0.3018 0.5502 0.073 Uiso 1 1 calc R U . . .
O103 O 0.5402(8) 0.0327(8) 0.5639(5) 0.088(4) Uani 1 1 d . . . . .
C5 C 0.7541(11) 0.0435(8) 0.3832(6) 0.061(4) Uani 1 1 d . . . . .
H5A H 0.7513 0.0835 0.3533 0.092 Uiso 1 1 calc R U . . .
H5B H 0.7201 0.0012 0.3722 0.092 Uiso 1 1 calc R U . . .
H5C H 0.8074 0.0251 0.3863 0.092 Uiso 1 1 calc R U . . .
C18 C 0.7971(10) 0.2656(9) 0.7686(7) 0.064(4) Uani 1 1 d . . . . .
H18A H 0.7728 0.2175 0.7569 0.097 Uiso 1 1 calc R U . . .
H18B H 0.7887 0.3040 0.7380 0.097 Uiso 1 1 calc R U . . .
H18C H 0.7740 0.2834 0.8054 0.097 Uiso 1 1 calc R U . . .
C2 C 0.6404(10) -0.0944(8) 0.4628(7) 0.060(4) Uani 1 1 d . . . . .
H2A H 0.6272 -0.1478 0.4552 0.090 Uiso 1 1 calc R U . . .
H2B H 0.6374 -0.0653 0.4262 0.090 Uiso 1 1 calc R U . . .
H2C H 0.6040 -0.0731 0.4913 0.090 Uiso 1 1 calc R U . . .
C1 C 0.7254(11) -0.1366(8) 0.5443(7) 0.070(5) Uani 1 1 d . . . . .
H1A H 0.6837 -0.1200 0.5704 0.106 Uiso 1 1 calc R U . . .
H1B H 0.7754 -0.1289 0.5637 0.106 Uiso 1 1 calc R U . . .
H1C H 0.7188 -0.1907 0.5351 0.106 Uiso 1 1 calc R U . . .
C23 C 1.0561(12) 0.2789(14) 0.6836(9) 0.102(7) Uani 1 1 d . . . . .
H23A H 1.0355 0.3201 0.7081 0.152 Uiso 1 1 calc R U . . .
H23B H 1.0367 0.2846 0.6435 0.152 Uiso 1 1 calc R U . . .
H23C H 1.1127 0.2813 0.6835 0.152 Uiso 1 1 calc R U . . .
C19 C 0.8945(11) 0.2114(9) 0.8351(6) 0.067(4) Uani 1 1 d . . . . .
H19A H 0.8792 0.2447 0.8676 0.100 Uiso 1 1 calc R U . . .
H19B H 0.9490 0.1972 0.8395 0.100 Uiso 1 1 calc R U . . .
H19C H 0.8624 0.1653 0.8355 0.100 Uiso 1 1 calc R U . . .
C202 C 0.9301(10) 0.0422(9) 0.7766(6) 0.056(2) Uani 1 1 d . . . . .
C22 C 1.0566(10) 0.1375(14) 0.6674(7) 0.090(7) Uani 1 1 d . . . . .
H22A H 1.0430 0.0879 0.6842 0.134 Uiso 1 1 calc R U . . .
H22B H 1.1128 0.1406 0.6623 0.134 Uiso 1 1 calc R U . . .
H22C H 1.0312 0.1434 0.6293 0.134 Uiso 1 1 calc R U . . .
C24 C 1.0663(12) 0.1878(12) 0.7675(7) 0.084(6) Uani 1 1 d . . . . .
H24A H 1.1208 0.1740 0.7622 0.127 Uiso 1 1 calc R U . . .
H24B H 1.0393 0.1463 0.7877 0.127 Uiso 1 1 calc R U . . .
H24C H 1.0628 0.2344 0.7909 0.127 Uiso 1 1 calc R U . . .
C21 C 1.0296(9) 0.2009(11) 0.7086(7) 0.065(4) 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
Ge1 N1 1.844(12) . ?
Ge1 N2 1.891(10) . ?
Ge1 Co1 2.413(3) . ?
Ge1 Co2 2.439(3) . ?
Co1 C103 1.78(2) . ?
Co1 C102 1.780(16) . ?
Co1 C101 1.787(16) . ?
Co1 P1 2.261(4) . ?
Co2 C203 1.74(2) . ?
Co2 C201 1.765(14) . ?
Co2 C202 1.761(15) . ?
Co2 P2 2.258(5) . ?
P1 C9 1.849(16) . ?
P1 C8 1.887(12) . ?
P1 C4 1.889(12) . ?
P2 C16 1.865(14) . ?
P2 C17 1.897(14) . ?
P2 C21 1.912(17) . ?
C102 O102 1.149(18) . ?
O101 C101 1.124(18) . ?
N2 C15 1.395(16) . ?
N2 C16 1.459(16) . ?
C4 C2 1.54(2) . ?
C4 C1 1.54(2) . ?
C4 C3 1.549(19) . ?
C203 O203 1.151(19) . ?
C9 N1 1.459(16) . ?
O202 C202 1.160(17) . ?
C10 N1 1.402(19) . ?
C10 C15 1.424(17) . ?
C10 C11 1.43(2) . ?
C17 C19 1.53(2) . ?
C17 C18 1.52(2) . ?
C17 C20 1.56(2) . ?
C8 C7 1.541(18) . ?
C8 C6 1.52(2) . ?
C8 C5 1.556(18) . ?
C11 C12 1.380(19) . ?
C13 C12 1.382(19) . ?
C13 C14 1.38(2) . ?
C201 O201 1.130(17) . ?
C15 C14 1.381(18) . ?
C103 O103 1.14(2) . ?
C23 C21 1.55(3) . ?
C22 C21 1.53(3) . ?
C24 C21 1.50(2) . ?

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 Ge1 N2 86.5(5) . . ?
N1 Ge1 Co1 102.7(4) . . ?
N2 Ge1 Co1 123.8(4) . . ?
N1 Ge1 Co2 123.3(4) . . ?
N2 Ge1 Co2 102.7(3) . . ?
Co1 Ge1 Co2 116.00(11) . . ?
C103 Co1 C102 94.2(8) . . ?
C103 Co1 C101 94.4(8) . . ?
C102 Co1 C101 123.5(7) . . ?
C103 Co1 P1 94.4(5) . . ?
C102 Co1 P1 110.3(5) . . ?
C101 Co1 P1 124.5(5) . . ?
C103 Co1 Ge1 174.2(5) . . ?
C102 Co1 Ge1 90.8(6) . . ?
C101 Co1 Ge1 80.3(6) . . ?
P1 Co1 Ge1 86.74(14) . . ?
C203 Co2 C201 118.7(8) . . ?
C203 Co2 C202 98.3(7) . . ?
C201 Co2 C202 90.1(6) . . ?
C203 Co2 P2 107.3(5) . . ?
C201 Co2 P2 132.2(6) . . ?
C202 Co2 P2 95.9(5) . . ?
C203 Co2 Ge1 96.8(5) . . ?
C201 Co2 Ge1 76.6(5) . . ?
C202 Co2 Ge1 163.4(5) . . ?
P2 Co2 Ge1 86.06(12) . . ?
C9 P1 C8 106.5(7) . . ?
C9 P1 C4 100.4(6) . . ?
C8 P1 C4 109.6(6) . . ?
C9 P1 Co1 109.7(5) . . ?
C8 P1 Co1 112.1(4) . . ?
C4 P1 Co1 117.4(5) . . ?
C16 P2 C17 102.6(7) . . ?
C16 P2 C21 104.3(7) . . ?
C17 P2 C21 109.7(8) . . ?
C16 P2 Co2 110.9(5) . . ?
C17 P2 Co2 114.5(5) . . ?
C21 P2 Co2 113.8(6) . . ?
O102 C102 Co1 175.9(15) . . ?
C15 N2 C16 121.8(11) . . ?
C15 N2 Ge1 112.2(8) . . ?
C16 N2 Ge1 117.2(9) . . ?
C2 C4 C1 107.9(13) . . ?
C2 C4 C3 109.7(12) . . ?
C1 C4 C3 107.8(12) . . ?
C2 C4 P1 111.3(9) . . ?
C1 C4 P1 107.1(10) . . ?
C3 C4 P1 112.9(10) . . ?
O203 C203 Co2 177.1(14) . . ?
N1 C9 P1 110.5(10) . . ?
N1 C10 C15 114.4(11) . . ?
N1 C10 C11 128.4(12) . . ?
C15 C10 C11 117.2(13) . . ?
C19 C17 C18 107.7(14) . . ?
C19 C17 C20 109.1(12) . . ?
C18 C17 C20 108.0(14) . . ?
C19 C17 P2 110.1(11) . . ?
C18 C17 P2 107.9(10) . . ?
C20 C17 P2 113.8(11) . . ?
O101 C101 Co1 178.8(17) . . ?
C10 N1 C9 118.3(11) . . ?
C10 N1 Ge1 113.1(8) . . ?
C9 N1 Ge1 120.8(10) . . ?
C7 C8 C6 107.4(11) . . ?
C7 C8 C5 106.7(12) . . ?
C6 C8 C5 110.0(12) . . ?
C7 C8 P1 107.8(9) . . ?
C6 C8 P1 111.1(10) . . ?
C5 C8 P1 113.5(9) . . ?
C12 C11 C10 120.3(13) . . ?
N2 C16 P2 110.4(9) . . ?
C12 C13 C14 119.4(13) . . ?
O201 C201 Co2 176.3(15) . . ?
C14 C15 N2 126.1(12) . . ?
C14 C15 C10 120.1(12) . . ?
N2 C15 C10 113.5(11) . . ?
C11 C12 C13 121.1(13) . . ?
O103 C103 Co1 176.6(15) . . ?
C15 C14 C13 121.5(12) . . ?
O202 C202 Co2 174.6(16) . . ?
C24 C21 C23 109.9(16) . . ?
C24 C21 C22 108.0(15) . . ?
C23 C21 C22 109.0(15) . . ?
C24 C21 P2 110.4(11) . . ?
C23 C21 P2 112.7(13) . . ?
C22 C21 P2 106.7(12) . . ?

_refine_diff_density_max         1.517
_refine_diff_density_min         -1.897
_refine_diff_density_rms         0.205

_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_6
_database_code_depnum_ccdc_archive 'CCDC 1516700'
_audit_update_record             
;
2016-11-11 deposited with the CCDC.
2016-12-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C24 H44 Cl2 Ge N2 P2 Pd), 2.5(C7 H8)'
_chemical_formula_sum            'C65.50 H108 Cl4 Ge2 N4 P4 Pd2'
_chemical_formula_weight         1575.21

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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.7387(6)
_cell_length_b                   17.2670(10)
_cell_length_c                   18.6974(10)
_cell_angle_alpha                74.296(5)
_cell_angle_beta                 80.993(4)
_cell_angle_gamma                80.308(4)
_cell_volume                     3571.6(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    149(2)
_cell_measurement_reflns_used    24113
_cell_measurement_theta_min      3.8340
_cell_measurement_theta_max      69.5330

_exptl_crystal_description       fragment
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_F_000             1626
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    7.499
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.43387
_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           
;
 One of the five toluene solvent molecules found in the crystal unit cell of 16064_lu390 was disordered
 about a center of symmetry and required restraints on its geometrical and thermal parameters.
;

_diffrn_ambient_temperature      149(2)
_diffrn_radiation_wavelength     1.54184
_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            43518
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.847
_diffrn_reflns_theta_max         69.811
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             13241
_reflns_number_gt                11788
_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, 2016)'
_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)+(0.0323P)²+1.5586P] 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         13241
_refine_ls_number_parameters     757
_refine_ls_number_restraints     99
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0265
_refine_ls_wR_factor_ref         0.0665
_refine_ls_wR_factor_gt          0.0633
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4473(3) 0.18286(19) 0.12747(19) 0.0489(7) Uani 1 1 d . . . . .
H1A H 0.4991 0.2002 0.1547 0.073 Uiso 1 1 calc R U . . .
H1B H 0.4216 0.2286 0.0867 0.073 Uiso 1 1 calc R U . . .
H1C H 0.4891 0.1382 0.1067 0.073 Uiso 1 1 calc R U . . .
C2 C 0.2722(3) 0.2250(2) 0.21054(19) 0.0536(8) Uani 1 1 d . . . . .
H2A H 0.3206 0.2431 0.2395 0.080 Uiso 1 1 calc R U . . .
H2B H 0.2023 0.2071 0.2427 0.080 Uiso 1 1 calc R U . . .
H2C H 0.2495 0.2700 0.1684 0.080 Uiso 1 1 calc R U . . .
C3 C 0.3825(3) 0.0868(2) 0.2474(2) 0.0621(9) Uani 1 1 d . . . . .
H3A H 0.4218 0.0395 0.2297 0.093 Uiso 1 1 calc R U . . .
H3B H 0.3153 0.0714 0.2837 0.093 Uiso 1 1 calc R U . . .
H3C H 0.4367 0.1064 0.2712 0.093 Uiso 1 1 calc R U . . .
C4 C 0.3414(2) 0.15414(17) 0.18092(16) 0.0408(6) Uani 1 1 d . . . . .
C5 C 0.1778(3) 0.26320(17) 0.04131(19) 0.0517(8) Uani 1 1 d . . . . .
H5A H 0.1539 0.2935 -0.0076 0.078 Uiso 1 1 calc R U . . .
H5B H 0.2430 0.2859 0.0513 0.078 Uiso 1 1 calc R U . . .
H5C H 0.1123 0.2674 0.0802 0.078 Uiso 1 1 calc R U . . .
C6 C 0.3211(3) 0.1685(2) -0.01741(17) 0.0528(8) Uani 1 1 d . . . . .
H6A H 0.3010 0.2011 -0.0665 0.079 Uiso 1 1 calc R U . . .
H6B H 0.3442 0.1117 -0.0192 0.079 Uiso 1 1 calc R U . . .
H6C H 0.3858 0.1889 -0.0040 0.079 Uiso 1 1 calc R U . . .
C7 C 0.1158(3) 0.1423(2) 0.01921(18) 0.0535(8) Uani 1 1 d . . . . .
H7A H 0.0452 0.1507 0.0533 0.080 Uiso 1 1 calc R U . . .
H7B H 0.1365 0.0842 0.0222 0.080 Uiso 1 1 calc R U . . .
H7C H 0.1019 0.1714 -0.0321 0.080 Uiso 1 1 calc R U . . .
C8 C 0.2154(3) 0.17421(17) 0.04128(15) 0.0401(6) Uani 1 1 d . . . . .
C9 C 0.3259(2) 0.01400(15) 0.11771(17) 0.0405(6) Uani 1 1 d . . . . .
H9A H 0.3175 0.0135 0.0660 0.049 Uiso 1 1 calc R U . . .
H9B H 0.4093 0.0144 0.1204 0.049 Uiso 1 1 calc R U . . .
C10 C 0.2554(2) -0.11765(14) 0.13719(15) 0.0320(5) Uani 1 1 d . . . . .
C11 C 0.3151(2) -0.14085(15) 0.07476(16) 0.0384(6) Uani 1 1 d . . . . .
H11 H 0.3838 -0.1183 0.0507 0.046 Uiso 1 1 calc R U . . .
C12 C 0.2748(3) -0.19696(17) 0.04705(17) 0.0435(6) Uani 1 1 d . . . . .
H12 H 0.3160 -0.2124 0.0040 0.052 Uiso 1 1 calc R U . . .
C13 C 0.1756(3) -0.23027(17) 0.08176(18) 0.0451(7) Uani 1 1 d . . . . .
H13 H 0.1485 -0.2684 0.0623 0.054 Uiso 1 1 calc R U . . .
C14 C 0.1147(2) -0.20871(15) 0.14499(17) 0.0401(6) Uani 1 1 d . . . . .
H14 H 0.0463 -0.2320 0.1686 0.048 Uiso 1 1 calc R U . . .
C15 C 0.1542(2) -0.15301(14) 0.17341(15) 0.0333(5) Uani 1 1 d . . . . .
C16 C -0.0228(2) -0.11897(15) 0.26077(17) 0.0399(6) Uani 1 1 d . . . . .
H16A H -0.0390 -0.1495 0.3135 0.048 Uiso 1 1 calc R U . . .
H16B H -0.0615 -0.1423 0.2296 0.048 Uiso 1 1 calc R U . . .
C17 C -0.0819(4) -0.0233(2) 0.39853(19) 0.0663(10) Uani 1 1 d . . . . .
H17A H -0.0313 0.0195 0.3826 0.099 Uiso 1 1 calc R U . . .
H17B H -0.0348 -0.0761 0.3997 0.099 Uiso 1 1 calc R U . . .
H17C H -0.1220 -0.0232 0.4486 0.099 Uiso 1 1 calc R U . . .
C18 C -0.2536(3) -0.0729(2) 0.3719(2) 0.0630(10) Uani 1 1 d . . . . .
H18A H -0.2108 -0.1260 0.3686 0.095 Uiso 1 1 calc R U . . .
H18B H -0.3177 -0.0593 0.3409 0.095 Uiso 1 1 calc R U . . .
H18C H -0.2850 -0.0749 0.4241 0.095 Uiso 1 1 calc R U . . .
C19 C -0.2402(4) 0.0759(2) 0.3408(3) 0.0906(16) Uani 1 1 d . . . . .
H19A H -0.2712 0.0800 0.3917 0.136 Uiso 1 1 calc R U . . .
H19B H -0.3046 0.0838 0.3109 0.136 Uiso 1 1 calc R U . . .
H19C H -0.1892 0.1177 0.3179 0.136 Uiso 1 1 calc R U . . .
C20 C -0.1708(3) -0.00793(17) 0.34395(18) 0.0493(8) Uani 1 1 d . . . . .
C21 C -0.0949(3) -0.0065(3) 0.1058(2) 0.0705(11) Uani 1 1 d . . . . .
H21A H -0.1341 0.0130 0.0604 0.106 Uiso 1 1 calc R U . . .
H21B H -0.0706 -0.0651 0.1146 0.106 Uiso 1 1 calc R U . . .
H21C H -0.0264 0.0213 0.0995 0.106 Uiso 1 1 calc R U . . .
C22 C -0.2747(3) -0.0437(2) 0.1883(2) 0.0593(9) Uani 1 1 d . . . . .
H22A H -0.3320 -0.0318 0.2294 0.089 Uiso 1 1 calc R U . . .
H22B H -0.2399 -0.1007 0.2022 0.089 Uiso 1 1 calc R U . . .
H22C H -0.3132 -0.0339 0.1432 0.089 Uiso 1 1 calc R U . . .
C23 C -0.2338(4) 0.0992(2) 0.1535(3) 0.0885(15) Uani 1 1 d . . . . .
H23A H -0.2730 0.1101 0.1085 0.133 Uiso 1 1 calc R U . . .
H23B H -0.1732 0.1346 0.1442 0.133 Uiso 1 1 calc R U . . .
H23C H -0.2907 0.1099 0.1952 0.133 Uiso 1 1 calc R U . . .
C24 C -0.1792(3) 0.01127(17) 0.17301(19) 0.0468(7) Uani 1 1 d . . . . .
C25 C 1.1558(2) 0.4267(2) 0.26637(19) 0.0499(7) Uani 1 1 d . . . . .
H25A H 1.1787 0.4479 0.2128 0.075 Uiso 1 1 calc R U . . .
H25B H 1.1271 0.3745 0.2748 0.075 Uiso 1 1 calc R U . . .
H25C H 1.2233 0.4191 0.2936 0.075 Uiso 1 1 calc R U . . .
C26 C 1.0348(2) 0.45795(19) 0.37937(16) 0.0427(6) Uani 1 1 d . . . . .
H26A H 1.1072 0.4500 0.4018 0.064 Uiso 1 1 calc R U . . .
H26B H 1.0023 0.4065 0.3925 0.064 Uiso 1 1 calc R U . . .
H26C H 0.9788 0.4988 0.3983 0.064 Uiso 1 1 calc R U . . .
C27 C 1.0997(3) 0.57095(19) 0.27615(18) 0.0467(7) Uani 1 1 d . . . . .
H27A H 1.1617 0.5689 0.3064 0.070 Uiso 1 1 calc R U . . .
H27B H 1.0339 0.6106 0.2874 0.070 Uiso 1 1 calc R U . . .
H27C H 1.1291 0.5870 0.2230 0.070 Uiso 1 1 calc R U . . .
C28 C 1.0596(2) 0.48690(16) 0.29439(15) 0.0341(5) Uani 1 1 d . . . . .
C29 C 0.9980(2) 0.43099(16) 0.12857(16) 0.0384(6) Uani 1 1 d . . . . .
H29A H 1.0023 0.4406 0.0742 0.058 Uiso 1 1 calc R U . . .
H29B H 0.9523 0.3865 0.1531 0.058 Uiso 1 1 calc R U . . .
H29C H 1.0767 0.4166 0.1435 0.058 Uiso 1 1 calc R U . . .
C30 C 1.0113(2) 0.57761(16) 0.11287(15) 0.0389(6) Uani 1 1 d . . . . .
H30A H 1.0096 0.5898 0.0587 0.058 Uiso 1 1 calc R U . . .
H30B H 1.0920 0.5613 0.1242 0.058 Uiso 1 1 calc R U . . .
H30C H 0.9784 0.6260 0.1307 0.058 Uiso 1 1 calc R U . . .
C31 C 0.8175(2) 0.53100(17) 0.12688(16) 0.0386(6) Uani 1 1 d . . . . .
H31A H 0.7819 0.5826 0.1380 0.058 Uiso 1 1 calc R U . . .
H31B H 0.7695 0.4884 0.1537 0.058 Uiso 1 1 calc R U . . .
H31C H 0.8231 0.5364 0.0729 0.058 Uiso 1 1 calc R U . . .
C32 C 0.9395(2) 0.50839(15) 0.15202(14) 0.0309(5) Uani 1 1 d . . . . .
C33 C 0.8684(2) 0.39231(15) 0.29315(15) 0.0331(5) Uani 1 1 d . . . . .
H33A H 0.8429 0.3768 0.2515 0.040 Uiso 1 1 calc R U . . .
H33B H 0.9351 0.3522 0.3110 0.040 Uiso 1 1 calc R U . . .
C34 C 0.6699(2) 0.36034(14) 0.34759(14) 0.0296(5) Uani 1 1 d . . . . .
C35 C 0.6674(2) 0.29550(15) 0.31754(16) 0.0375(6) Uani 1 1 d . . . . .
H35 H 0.7379 0.2666 0.3003 0.045 Uiso 1 1 calc R U . . .
C36 C 0.5608(3) 0.27317(17) 0.31283(18) 0.0438(7) Uani 1 1 d . . . . .
H36 H 0.5591 0.2293 0.2916 0.053 Uiso 1 1 calc R U . . .
C37 C 0.4581(2) 0.31362(17) 0.33843(17) 0.0425(7) Uani 1 1 d . . . . .
H37 H 0.3861 0.2975 0.3349 0.051 Uiso 1 1 calc R U . . .
C38 C 0.4591(2) 0.37816(15) 0.36950(15) 0.0353(6) Uani 1 1 d . . . . .
H38 H 0.3880 0.4055 0.3878 0.042 Uiso 1 1 calc R U . . .
C39 C 0.5641(2) 0.40270(14) 0.37386(14) 0.0292(5) Uani 1 1 d . . . . .
C40 C 0.4972(2) 0.54321(14) 0.39528(14) 0.0296(5) Uani 1 1 d . . . . .
H40A H 0.4764 0.5564 0.4444 0.035 Uiso 1 1 calc R U . . .
H40B H 0.4246 0.5366 0.3781 0.035 Uiso 1 1 calc R U . . .
C41 C 0.6195(3) 0.6975(2) 0.42812(19) 0.0537(8) Uani 1 1 d . . . . .
H41A H 0.6039 0.7377 0.4579 0.080 Uiso 1 1 calc R U . . .
H41B H 0.6969 0.7005 0.3997 0.080 Uiso 1 1 calc R U . . .
H41C H 0.6164 0.6431 0.4614 0.080 Uiso 1 1 calc R U . . .
C42 C 0.5417(3) 0.79674(17) 0.31718(19) 0.0505(8) Uani 1 1 d . . . . .
H42A H 0.5388 0.8389 0.3438 0.076 Uiso 1 1 calc R U . . .
H42B H 0.4785 0.8111 0.2855 0.076 Uiso 1 1 calc R U . . .
H42C H 0.6166 0.7924 0.2860 0.076 Uiso 1 1 calc R U . . .
C43 C 0.4063(2) 0.71881(17) 0.41878(17) 0.0439(7) Uani 1 1 d . . . . .
H43A H 0.3994 0.6673 0.4563 0.066 Uiso 1 1 calc R U . . .
H43B H 0.3470 0.7285 0.3847 0.066 Uiso 1 1 calc R U . . .
H43C H 0.3951 0.7631 0.4438 0.066 Uiso 1 1 calc R U . . .
C44 C 0.5280(2) 0.71508(16) 0.37404(16) 0.0378(6) Uani 1 1 d . . . . .
C45 C 0.4918(3) 0.56700(17) 0.22337(16) 0.0425(6) Uani 1 1 d . . . . .
H45A H 0.4603 0.5752 0.1760 0.064 Uiso 1 1 calc R U . . .
H45B H 0.4478 0.5300 0.2631 0.064 Uiso 1 1 calc R U . . .
H45C H 0.5738 0.5435 0.2186 0.064 Uiso 1 1 calc R U . . .
C46 C 0.3532(2) 0.68060(18) 0.25981(17) 0.0438(7) Uani 1 1 d . . . . .
H46A H 0.3467 0.7348 0.2684 0.066 Uiso 1 1 calc R U . . .
H46B H 0.3189 0.6438 0.3046 0.066 Uiso 1 1 calc R U . . .
H46C H 0.3119 0.6836 0.2173 0.066 Uiso 1 1 calc R U . . .
C47 C 0.5359(3) 0.70815(18) 0.17466(16) 0.0437(7) Uani 1 1 d . . . . .
H47A H 0.6174 0.6870 0.1625 0.066 Uiso 1 1 calc R U . . .
H47B H 0.5318 0.7609 0.1859 0.066 Uiso 1 1 calc R U . . .
H47C H 0.4931 0.7147 0.1319 0.066 Uiso 1 1 calc R U . . .
C48 C 0.4817(2) 0.64868(16) 0.24284(15) 0.0351(6) Uani 1 1 d . . . . .
C49 C 0.2633(3) 0.6528(2) 0.9310(2) 0.0657(10) Uani 1 1 d . . . . .
H49A H 0.2443 0.6632 0.8798 0.099 Uiso 1 1 calc R U . . .
H49B H 0.2413 0.7025 0.9485 0.099 Uiso 1 1 calc R U . . .
H49C H 0.2206 0.6098 0.9638 0.099 Uiso 1 1 calc R U . . .
C50 C 0.3901(3) 0.62680(18) 0.93253(18) 0.0471(7) Uani 1 1 d . . . . .
C51 C 0.4439(3) 0.61930(18) 0.99609(17) 0.0468(7) Uani 1 1 d . . . . .
H51 H 0.3984 0.6314 1.0394 0.056 Uiso 1 1 calc R U . . .
C52 C 0.5616(3) 0.59476(18) 0.99737(19) 0.0508(7) Uani 1 1 d . . . . .
H52 H 0.5965 0.5900 1.0412 0.061 Uiso 1 1 calc R U . . .
C53 C 0.6287(3) 0.5771(2) 0.9350(2) 0.0579(9) Uani 1 1 d . . . . .
H53 H 0.7099 0.5602 0.9355 0.070 Uiso 1 1 calc R U . . .
C54 C 0.5768(3) 0.5841(2) 0.8720(2) 0.0629(10) Uani 1 1 d . . . . .
H54 H 0.6228 0.5719 0.8289 0.075 Uiso 1 1 calc R U . . .
C55 C 0.4597(3) 0.6083(2) 0.87072(18) 0.0540(8) Uani 1 1 d . . . . .
H55 H 0.4256 0.6126 0.8267 0.065 Uiso 1 1 calc R U . . .
C56 C 0.0218(5) 0.3095(3) 0.5788(3) 0.0875(14) Uani 1 1 d . . . . .
H56A H 0.0248 0.3673 0.5553 0.131 Uiso 1 1 calc R U . . .
H56B H 0.0882 0.2873 0.6074 0.131 Uiso 1 1 calc R U . . .
H56C H -0.0508 0.3028 0.6124 0.131 Uiso 1 1 calc R U . . .
C57 C 0.0263(3) 0.26571(19) 0.52017(19) 0.0564(8) Uani 1 1 d . . . . .
C58 C -0.0721(3) 0.2459(2) 0.5023(2) 0.0647(10) Uani 1 1 d . . . . .
H58 H -0.1453 0.2580 0.5296 0.078 Uiso 1 1 calc R U . . .
C59 C -0.0662(4) 0.2080(2) 0.4445(3) 0.0745(11) Uani 1 1 d . . . . .
H59 H -0.1351 0.1949 0.4325 0.089 Uiso 1 1 calc R U . . .
C60 C 0.0374(4) 0.1900(2) 0.4054(2) 0.0747(11) Uani 1 1 d . . . . .
H60 H 0.0413 0.1639 0.3662 0.090 Uiso 1 1 calc R U . . .
C61 C 0.1360(4) 0.2092(2) 0.4223(2) 0.0720(10) Uani 1 1 d . . . . .
H61 H 0.2087 0.1964 0.3948 0.086 Uiso 1 1 calc R U . . .
C62 C 0.1314(3) 0.2468(2) 0.4788(2) 0.0629(9) Uani 1 1 d . . . . .
H62 H 0.2010 0.2601 0.4898 0.076 Uiso 1 1 calc R U . . .
C64 C 0.4530(10) -0.1187(6) 0.5046(6) 0.0888(13) Uani 0.5 1 d D U P A -1
H64A H 0.3715 -0.1159 0.4969 0.133 Uiso 0.5 1 calc R U P A -1
H64B H 0.4671 -0.1557 0.5533 0.133 Uiso 0.5 1 calc R U P A -1
H64C H 0.5040 -0.1387 0.4649 0.133 Uiso 0.5 1 calc R U P A -1
C65 C 0.4763(8) -0.0402(5) 0.5029(5) 0.0888(13) Uani 0.5 1 d D U P A -1
C66 C 0.5543(10) -0.0206(6) 0.5437(6) 0.0888(13) Uani 0.5 1 d D U P A -1
H66 H 0.5943 -0.0608 0.5802 0.107 Uiso 0.5 1 calc R U P A -1
C67 C 0.5690(8) 0.0586(6) 0.5280(5) 0.0888(13) Uani 0.5 1 d D U P A -1
H67 H 0.6235 0.0741 0.5523 0.107 Uiso 0.5 1 calc R U P A -1
C68 C 0.5037(9) 0.1199(6) 0.4754(5) 0.0888(13) Uani 0.5 1 d D U P A -1
H68 H 0.5095 0.1756 0.4690 0.107 Uiso 0.5 1 calc R U P A -1
C69 C 0.4380(8) 0.0992(6) 0.4372(5) 0.0888(13) Uani 0.5 1 d D U P A -1
H69 H 0.4016 0.1395 0.3990 0.107 Uiso 0.5 1 calc R U P A -1
C70 C 0.4186(10) 0.0184(7) 0.4506(6) 0.0888(13) Uani 0.5 1 d D U P A -1
H70 H 0.3661 0.0044 0.4238 0.107 Uiso 0.5 1 calc R U P A -1
Cl1 Cl 0.23674(7) -0.08001(5) 0.35258(4) 0.05188(18) Uani 1 1 d . . . . .
Cl2 Cl -0.04591(6) 0.21097(4) 0.20005(5) 0.04844(17) Uani 1 1 d . . . . .
Cl3 Cl 0.77842(5) 0.47529(4) 0.49558(3) 0.03907(14) Uani 1 1 d . . . . .
Cl4 Cl 0.81976(5) 0.71782(3) 0.20720(4) 0.03596(13) Uani 1 1 d . . . . .
Ge1 Ge 0.17355(2) -0.04434(2) 0.24434(2) 0.03097(7) Uani 1 1 d . . . . .
Ge2 Ge 0.72951(2) 0.48252(2) 0.38589(2) 0.02530(6) Uani 1 1 d . . . . .
N1 N 0.28926(18) -0.06029(12) 0.16886(13) 0.0339(5) Uani 1 1 d . . . . .
N2 N 0.10232(18) -0.12874(12) 0.23837(13) 0.0352(5) Uani 1 1 d . . . . .
N3 N 0.77337(16) 0.38879(12) 0.35387(11) 0.0278(4) Uani 1 1 d . . . . .
N4 N 0.57555(17) 0.46666(11) 0.40424(11) 0.0276(4) Uani 1 1 d . . . . .
P1 P 0.24009(5) 0.11054(4) 0.13837(4) 0.02976(13) Uani 1 1 d . . . . .
P2 P -0.08620(5) -0.00843(4) 0.25074(4) 0.03288(14) Uani 1 1 d . . . . .
P3 P 0.91811(5) 0.49607(3) 0.25661(3) 0.02595(12) Uani 1 1 d . . . . .
P4 P 0.56418(5) 0.63072(3) 0.32580(3) 0.02646(12) Uani 1 1 d . . . . .
Pd1 Pd 0.06259(2) 0.07854(2) 0.21177(2) 0.02817(5) Uani 1 1 d . . . . .
Pd2 Pd 0.76608(2) 0.59352(2) 0.29080(2) 0.02442(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C4 1.530(4) . ?
C2 C4 1.534(4) . ?
C3 C4 1.532(4) . ?
C4 P1 1.881(3) . ?
C5 C8 1.526(4) . ?
C6 C8 1.532(4) . ?
C7 C8 1.527(4) . ?
C8 P1 1.888(3) . ?
C9 N1 1.462(3) . ?
C9 P1 1.898(3) . ?
C10 C11 1.384(4) . ?
C10 C15 1.418(4) . ?
C10 N1 1.419(3) . ?
C11 C12 1.390(4) . ?
C12 C13 1.377(4) . ?
C13 C14 1.390(4) . ?
C14 C15 1.388(4) . ?
C15 N2 1.407(4) . ?
C16 N2 1.457(3) . ?
C16 P2 1.898(3) . ?
C17 C20 1.515(5) . ?
C18 C20 1.538(4) . ?
C19 C20 1.528(5) . ?
C20 P2 1.867(3) . ?
C21 C24 1.540(5) . ?
C22 C24 1.533(4) . ?
C23 C24 1.515(5) . ?
C24 P2 1.877(3) . ?
C25 C28 1.531(4) . ?
C26 C28 1.528(4) . ?
C27 C28 1.535(4) . ?
C28 P3 1.872(3) . ?
C29 C32 1.537(3) . ?
C30 C32 1.532(3) . ?
C31 C32 1.533(4) . ?
C32 P3 1.890(3) . ?
C33 N3 1.458(3) . ?
C33 P3 1.893(2) . ?
C34 C35 1.388(4) . ?
C34 N3 1.417(3) . ?
C34 C39 1.420(4) . ?
C35 C36 1.392(4) . ?
C36 C37 1.374(4) . ?
C37 C38 1.392(4) . ?
C38 C39 1.390(3) . ?
C39 N4 1.405(3) . ?
C40 N4 1.463(3) . ?
C40 P4 1.899(2) . ?
C41 C44 1.527(4) . ?
C42 C44 1.535(4) . ?
C43 C44 1.539(4) . ?
C44 P4 1.870(3) . ?
C45 C48 1.531(4) . ?
C46 C48 1.531(4) . ?
C47 C48 1.530(4) . ?
C48 P4 1.884(3) . ?
C49 C50 1.482(5) . ?
C50 C55 1.386(5) . ?
C50 C51 1.398(4) . ?
C51 C52 1.377(5) . ?
C52 C53 1.377(5) . ?
C53 C54 1.377(5) . ?
C54 C55 1.371(5) . ?
C56 C57 1.480(5) . ?
C57 C58 1.371(5) . ?
C57 C62 1.389(5) . ?
C58 C59 1.393(6) . ?
C59 C60 1.352(6) . ?
C60 C61 1.361(6) . ?
C61 C62 1.372(6) . ?
C64 C65 1.417(11) . ?
C65 C70 1.372(9) . ?
C65 C66 1.414(13) . ?
C66 C67 1.353(9) . ?
C67 C68 1.440(13) . ?
C68 C69 1.278(8) . ?
C69 C70 1.400(14) . ?
Cl1 Ge1 2.1604(8) . ?
Cl2 Pd1 2.3946(7) . ?
Cl3 Ge2 2.1812(7) . ?
Cl4 Pd2 2.4036(6) . ?
Ge1 N2 1.834(2) . ?
Ge1 N1 1.843(2) . ?
Ge1 Pd1 2.2777(3) . ?
Ge2 N4 1.8386(19) . ?
Ge2 N3 1.841(2) . ?
Ge2 Pd2 2.2831(3) . ?
P1 Pd1 2.3689(6) . ?
P2 Pd1 2.3936(6) . ?
P3 Pd2 2.3747(6) . ?
P4 Pd2 2.3848(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 C4 C3 109.3(3) . . ?
C1 C4 C2 109.7(2) . . ?
C3 C4 C2 108.5(3) . . ?
C1 C4 P1 114.3(2) . . ?
C3 C4 P1 106.30(19) . . ?
C2 C4 P1 108.5(2) . . ?
C5 C8 C7 108.4(3) . . ?
C5 C8 C6 108.8(2) . . ?
C7 C8 C6 108.5(3) . . ?
C5 C8 P1 110.9(2) . . ?
C7 C8 P1 105.94(18) . . ?
C6 C8 P1 114.0(2) . . ?
N1 C9 P1 113.77(18) . . ?
C11 C10 C15 119.3(2) . . ?
C11 C10 N1 124.2(2) . . ?
C15 C10 N1 116.5(2) . . ?
C10 C11 C12 120.3(2) . . ?
C13 C12 C11 120.2(3) . . ?
C12 C13 C14 120.7(3) . . ?
C15 C14 C13 119.7(3) . . ?
C14 C15 N2 124.8(2) . . ?
C14 C15 C10 119.8(3) . . ?
N2 C15 C10 115.4(2) . . ?
N2 C16 P2 112.20(17) . . ?
C17 C20 C19 108.6(3) . . ?
C17 C20 C18 108.9(3) . . ?
C19 C20 C18 109.5(3) . . ?
C17 C20 P2 106.2(2) . . ?
C19 C20 P2 109.4(2) . . ?
C18 C20 P2 114.2(2) . . ?
C23 C24 C22 109.2(3) . . ?
C23 C24 C21 109.3(3) . . ?
C22 C24 C21 107.6(3) . . ?
C23 C24 P2 110.8(2) . . ?
C22 C24 P2 114.6(2) . . ?
C21 C24 P2 105.0(2) . . ?
C26 C28 C25 108.9(2) . . ?
C26 C28 C27 107.7(2) . . ?
C25 C28 C27 110.3(2) . . ?
C26 C28 P3 106.28(17) . . ?
C25 C28 P3 113.93(19) . . ?
C27 C28 P3 109.51(19) . . ?
C30 C32 C31 108.8(2) . . ?
C30 C32 C29 108.9(2) . . ?
C31 C32 C29 108.8(2) . . ?
C30 C32 P3 110.57(17) . . ?
C31 C32 P3 105.90(17) . . ?
C29 C32 P3 113.71(18) . . ?
N3 C33 P3 113.34(17) . . ?
C35 C34 N3 124.1(2) . . ?
C35 C34 C39 119.8(2) . . ?
N3 C34 C39 116.1(2) . . ?
C34 C35 C36 119.5(3) . . ?
C37 C36 C35 121.0(3) . . ?
C36 C37 C38 120.2(2) . . ?
C39 C38 C37 120.1(3) . . ?
C38 C39 N4 125.0(2) . . ?
C38 C39 C34 119.3(2) . . ?
N4 C39 C34 115.7(2) . . ?
N4 C40 P4 112.54(15) . . ?
C41 C44 C42 109.0(2) . . ?
C41 C44 C43 108.9(2) . . ?
C42 C44 C43 110.0(2) . . ?
C41 C44 P4 104.35(19) . . ?
C42 C44 P4 110.0(2) . . ?
C43 C44 P4 114.39(19) . . ?
C47 C48 C46 109.2(2) . . ?
C47 C48 C45 107.7(2) . . ?
C46 C48 C45 109.6(2) . . ?
C47 C48 P4 111.27(18) . . ?
C46 C48 P4 112.1(2) . . ?
C45 C48 P4 106.86(18) . . ?
C55 C50 C51 117.4(3) . . ?
C55 C50 C49 121.0(3) . . ?
C51 C50 C49 121.6(3) . . ?
C52 C51 C50 121.4(3) . . ?
C51 C52 C53 119.9(3) . . ?
C54 C53 C52 119.4(3) . . ?
C55 C54 C53 120.8(3) . . ?
C54 C55 C50 121.1(3) . . ?
C58 C57 C62 117.7(4) . . ?
C58 C57 C56 121.9(4) . . ?
C62 C57 C56 120.2(4) . . ?
C57 C58 C59 120.8(4) . . ?
C60 C59 C58 120.2(4) . . ?
C59 C60 C61 119.8(4) . . ?
C60 C61 C62 120.6(4) . . ?
C61 C62 C57 120.8(4) . . ?
C70 C65 C66 121.2(9) . . ?
C70 C65 C64 111.2(9) . . ?
C66 C65 C64 127.4(8) . . ?
C67 C66 C65 116.5(9) . . ?
C66 C67 C68 121.5(8) . . ?
C69 C68 C67 120.0(9) . . ?
C68 C69 C70 121.3(9) . . ?
C65 C70 C69 119.2(9) . . ?
N2 Ge1 N1 92.47(9) . . ?
N2 Ge1 Cl1 106.14(8) . . ?
N1 Ge1 Cl1 112.18(7) . . ?
N2 Ge1 Pd1 113.06(7) . . ?
N1 Ge1 Pd1 111.75(7) . . ?
Cl1 Ge1 Pd1 118.20(3) . . ?
N4 Ge2 N3 92.25(8) . . ?
N4 Ge2 Cl3 104.46(7) . . ?
N3 Ge2 Cl3 114.48(7) . . ?
N4 Ge2 Pd2 113.56(6) . . ?
N3 Ge2 Pd2 110.65(6) . . ?
Cl3 Ge2 Pd2 118.30(2) . . ?
C10 N1 C9 117.6(2) . . ?
C10 N1 Ge1 106.54(15) . . ?
C9 N1 Ge1 114.95(16) . . ?
C15 N2 C16 123.7(2) . . ?
C15 N2 Ge1 107.75(15) . . ?
C16 N2 Ge1 113.67(17) . . ?
C34 N3 C33 119.3(2) . . ?
C34 N3 Ge2 107.03(15) . . ?
C33 N3 Ge2 115.33(15) . . ?
C39 N4 C40 124.6(2) . . ?
C39 N4 Ge2 107.69(15) . . ?
C40 N4 Ge2 112.22(14) . . ?
C4 P1 C8 111.22(12) . . ?
C4 P1 C9 105.51(13) . . ?
C8 P1 C9 101.59(13) . . ?
C4 P1 Pd1 116.98(9) . . ?
C8 P1 Pd1 111.55(9) . . ?
C9 P1 Pd1 108.61(8) . . ?
C20 P2 C24 113.87(15) . . ?
C20 P2 C16 103.62(13) . . ?
C24 P2 C16 102.54(14) . . ?
C20 P2 Pd1 115.79(11) . . ?
C24 P2 Pd1 108.74(9) . . ?
C16 P2 Pd1 111.40(8) . . ?
C28 P3 C32 111.57(11) . . ?
C28 P3 C33 105.53(12) . . ?
C32 P3 C33 102.39(11) . . ?
C28 P3 Pd2 116.72(9) . . ?
C32 P3 Pd2 111.11(8) . . ?
C33 P3 Pd2 108.30(8) . . ?
C44 P4 C48 112.80(13) . . ?
C44 P4 C40 103.58(11) . . ?
C48 P4 C40 102.56(11) . . ?
C44 P4 Pd2 115.81(8) . . ?
C48 P4 Pd2 109.68(9) . . ?
C40 P4 Pd2 111.47(8) . . ?
Ge1 Pd1 P1 80.604(18) . . ?
Ge1 Pd1 P2 79.793(18) . . ?
P1 Pd1 P2 149.36(2) . . ?
Ge1 Pd1 Cl2 168.84(2) . . ?
P1 Pd1 Cl2 101.04(2) . . ?
P2 Pd1 Cl2 102.75(2) . . ?
Ge2 Pd2 P3 80.125(17) . . ?
Ge2 Pd2 P4 80.121(17) . . ?
P3 Pd2 P4 148.99(2) . . ?
Ge2 Pd2 Cl4 169.595(19) . . ?
P3 Pd2 Cl4 101.94(2) . . ?
P4 Pd2 Cl4 101.81(2) . . ?

_refine_diff_density_max         0.601
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.062

_shelxl_version_number           2014-3



#===END
#-----------------------------------------------------------------------------80

# End of file

