# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_NL-51
_database_code_depnum_ccdc_archive 'CCDC 1855503'
_audit_update_record             
;
2018-07-12 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C54 H60 Cl2 Ge N2 O P2 Ru S'
_chemical_formula_sum            'C54 H60 Cl2 Ge N2 O P2 Ru S'
_chemical_formula_weight         1091.62
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.5612(6)
_cell_length_b                   24.1634(10)
_cell_length_c                   16.9752(9)
_cell_angle_alpha                90
_cell_angle_beta                 96.627(2)
_cell_angle_gamma                90
_cell_volume                     5117.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    4885
_cell_measurement_theta_min      3.5
_cell_measurement_theta_max      24.93
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2248
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.13
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_absorpt_correction_T_min  0.6817
_exptl_absorpt_correction_T_max  0.7454

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_measurement_device_type  'Bruker Kappa APEX II Quazar'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.1056
_diffrn_reflns_av_unetI/netI     0.0863
_diffrn_reflns_number            58061
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.45
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_full        25.35
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_reflns_number_total             9335
_reflns_number_gt                6320
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       APEX2
_computing_cell_refinement       'APEX2 and SAINT'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0549P)²+0.9437P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         9335
_refine_ls_number_parameters     584
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0446
_refine_ls_wR_factor_ref         0.1195
_refine_ls_wR_factor_gt          0.0996
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.115

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3574(4) 0.58472(18) 0.7583(3) 0.0249(11) Uani 1 1 d . . .
H1A H 0.3381 0.6063 0.8042 0.03 Uiso 1 1 calc R . .
H1B H 0.291 0.5753 0.7237 0.03 Uiso 1 1 calc R . .
C2 C 0.3396(4) 0.46978(19) 0.7515(3) 0.0286(13) Uani 1 1 d . . .
C3 C 0.3677(5) 0.4351(2) 0.6938(4) 0.0394(15) Uani 1 1 d . . .
H3 H 0.4335 0.44 0.6721 0.047 Uiso 1 1 calc R . .
C4 C 0.2990(5) 0.3929(2) 0.6678(4) 0.0546(19) Uani 1 1 d . . .
H4 H 0.3159 0.369 0.6265 0.066 Uiso 1 1 calc R . .
C5 C 0.2062(6) 0.3854(3) 0.7013(5) 0.068(2) Uani 1 1 d . . .
H5 H 0.1608 0.3551 0.6845 0.082 Uiso 1 1 calc R . .
C6 C 0.1775(5) 0.4203(3) 0.7583(5) 0.070(2) Uani 1 1 d . . .
H6 H 0.1115 0.4156 0.7797 0.084 Uiso 1 1 calc R . .
C7 C 0.2463(5) 0.4625(2) 0.7841(4) 0.0536(18) Uani 1 1 d . . .
H7 H 0.2287 0.4867 0.8248 0.064 Uiso 1 1 calc R . .
C8 C 0.3291(4) 0.68913(18) 0.6225(3) 0.0230(11) Uani 1 1 d . . .
C9 C 0.3292(4) 0.6032(2) 0.5288(3) 0.0285(12) Uani 1 1 d . . .
H9 H 0.2536 0.6121 0.5073 0.034 Uiso 1 1 calc R . .
C10 C 0.3340(4) 0.5432(2) 0.5598(3) 0.0344(14) Uani 1 1 d . . .
H10A H 0.4063 0.5353 0.5855 0.052 Uiso 1 1 calc R . .
H10B H 0.3166 0.5176 0.5153 0.052 Uiso 1 1 calc R . .
H10C H 0.2821 0.5385 0.5982 0.052 Uiso 1 1 calc R . .
C11 C 0.4007(5) 0.6104(2) 0.4637(3) 0.0402(14) Uani 1 1 d . . .
H11A H 0.401 0.6494 0.4479 0.06 Uiso 1 1 calc R . .
H11B H 0.3735 0.5877 0.4179 0.06 Uiso 1 1 calc R . .
H11C H 0.4738 0.5988 0.4832 0.06 Uiso 1 1 calc R . .
C12 C 0.3838(4) 0.7455(2) 0.7475(3) 0.0320(13) Uani 1 1 d . . .
H12 H 0.3307 0.7736 0.7243 0.038 Uiso 1 1 calc R . .
C13 C 0.3523(6) 0.7268(2) 0.8270(4) 0.0599(19) Uani 1 1 d . . .
H13A H 0.281 0.7098 0.8192 0.09 Uiso 1 1 calc R . .
H13B H 0.3509 0.7588 0.8623 0.09 Uiso 1 1 calc R . .
H13C H 0.4045 0.6997 0.8507 0.09 Uiso 1 1 calc R . .
C14 C 0.4937(5) 0.7713(2) 0.7570(4) 0.0482(17) Uani 1 1 d . . .
H14A H 0.546 0.7444 0.7813 0.072 Uiso 1 1 calc R . .
H14B H 0.4936 0.8041 0.7909 0.072 Uiso 1 1 calc R . .
H14C H 0.513 0.782 0.7048 0.072 Uiso 1 1 calc R . .
C15 C 0.2456(4) 0.72792(19) 0.5801(3) 0.0287(12) Uani 1 1 d . . .
C16 C 0.1950(4) 0.7085(2) 0.5001(4) 0.0427(15) Uani 1 1 d . . .
H16A H 0.2512 0.6972 0.4679 0.064 Uiso 1 1 calc R . .
H16B H 0.153 0.7387 0.4734 0.064 Uiso 1 1 calc R . .
H16C H 0.1478 0.6769 0.5069 0.064 Uiso 1 1 calc R . .
C17 C 0.1531(4) 0.7344(2) 0.6317(4) 0.0447(16) Uani 1 1 d . . .
H17A H 0.1207 0.6981 0.6392 0.067 Uiso 1 1 calc R . .
H17B H 0.0988 0.7594 0.6053 0.067 Uiso 1 1 calc R . .
H17C H 0.1809 0.7498 0.6834 0.067 Uiso 1 1 calc R . .
C18 C 0.3003(5) 0.7837(2) 0.5667(4) 0.0519(18) Uani 1 1 d . . .
H18A H 0.3329 0.7984 0.6177 0.078 Uiso 1 1 calc R . .
H18B H 0.2469 0.81 0.5424 0.078 Uiso 1 1 calc R . .
H18C H 0.356 0.7782 0.5315 0.078 Uiso 1 1 calc R . .
C19 C 0.6971(4) 0.70884(18) 0.6405(3) 0.0221(11) Uani 1 1 d . . .
C20 C 0.6201(4) 0.6956(2) 0.5786(3) 0.0277(12) Uani 1 1 d . . .
H20 H 0.5948 0.6586 0.573 0.033 Uiso 1 1 calc R . .
C21 C 0.5791(4) 0.7352(2) 0.5247(3) 0.0365(14) Uani 1 1 d . . .
H21 H 0.5272 0.7249 0.482 0.044 Uiso 1 1 calc R . .
C22 C 0.6124(5) 0.7889(2) 0.5319(4) 0.0449(16) Uani 1 1 d . . .
H22 H 0.5832 0.816 0.495 0.054 Uiso 1 1 calc R . .
C23 C 0.6893(5) 0.8036(2) 0.5935(4) 0.0466(17) Uani 1 1 d . . .
H23 H 0.7134 0.8408 0.5991 0.056 Uiso 1 1 calc R . .
C24 C 0.7308(4) 0.7635(2) 0.6469(3) 0.0363(14) Uani 1 1 d . . .
H24 H 0.7836 0.7737 0.689 0.044 Uiso 1 1 calc R . .
C25 C 0.8211(4) 0.69734(17) 0.7893(3) 0.0212(11) Uani 1 1 d . . .
C26 C 0.7663(4) 0.71475(18) 0.8518(3) 0.0240(12) Uani 1 1 d . . .
H26 H 0.6939 0.7038 0.8534 0.029 Uiso 1 1 calc R . .
C27 C 0.8164(4) 0.74799(19) 0.9117(3) 0.0300(13) Uani 1 1 d . . .
H27 H 0.7779 0.7596 0.9537 0.036 Uiso 1 1 calc R . .
C28 C 0.9212(4) 0.7643(2) 0.9108(3) 0.0320(13) Uani 1 1 d . . .
H28 H 0.9557 0.7861 0.9529 0.038 Uiso 1 1 calc R . .
C29 C 0.9756(4) 0.74869(19) 0.8483(3) 0.0329(14) Uani 1 1 d . . .
H29 H 1.0477 0.7602 0.847 0.039 Uiso 1 1 calc R . .
C30 C 0.9258(4) 0.71635(18) 0.7876(3) 0.0279(12) Uani 1 1 d . . .
H30 H 0.9634 0.7069 0.744 0.033 Uiso 1 1 calc R . .
C31 C 0.8643(4) 0.62761(18) 0.6605(3) 0.0208(11) Uani 1 1 d . . .
C32 C 0.9542(4) 0.60524(19) 0.7056(3) 0.0249(12) Uani 1 1 d . . .
H32 H 0.9606 0.6076 0.7619 0.03 Uiso 1 1 calc R . .
C33 C 1.0331(4) 0.5800(2) 0.6691(4) 0.0346(14) Uani 1 1 d . . .
H33 H 1.0936 0.5646 0.7004 0.042 Uiso 1 1 calc R . .
C34 C 1.0258(4) 0.5765(2) 0.5875(4) 0.0390(15) Uani 1 1 d . . .
H34 H 1.0809 0.5591 0.5627 0.047 Uiso 1 1 calc R . .
C35 C 0.9372(4) 0.5988(2) 0.5418(3) 0.0361(14) Uani 1 1 d . . .
H35 H 0.931 0.5962 0.4856 0.043 Uiso 1 1 calc R . .
C36 C 0.8585(4) 0.62458(19) 0.5784(3) 0.0299(13) Uani 1 1 d . . .
H36 H 0.7991 0.6406 0.5469 0.036 Uiso 1 1 calc R . .
C37 C 0.8738(4) 0.54603(19) 0.8688(3) 0.0241(12) Uani 1 1 d . . .
C38 C 0.8630(4) 0.5922(2) 0.9161(3) 0.0310(13) Uani 1 1 d . . .
H38 H 0.7957 0.6104 0.9135 0.037 Uiso 1 1 calc R . .
C39 C 0.9478(5) 0.6118(2) 0.9663(4) 0.0457(16) Uani 1 1 d . . .
H39 H 0.9385 0.6433 0.9985 0.055 Uiso 1 1 calc R . .
C40 C 1.0464(5) 0.5864(3) 0.9706(4) 0.0485(17) Uani 1 1 d . . .
H40 H 1.1051 0.6004 1.0051 0.058 Uiso 1 1 calc R . .
C41 C 1.0591(4) 0.5411(3) 0.9252(4) 0.0444(16) Uani 1 1 d . . .
H41 H 1.1269 0.5233 0.9288 0.053 Uiso 1 1 calc R . .
C42 C 0.9745(4) 0.5206(2) 0.8738(3) 0.0337(13) Uani 1 1 d . . .
H42 H 0.985 0.4892 0.8419 0.04 Uiso 1 1 calc R . .
C43 C 0.8181(4) 0.46716(18) 0.7453(3) 0.0229(11) Uani 1 1 d . . .
C44 C 0.8441(4) 0.47860(19) 0.6702(3) 0.0228(11) Uani 1 1 d . . .
H44 H 0.8282 0.5141 0.6477 0.027 Uiso 1 1 calc R . .
C45 C 0.8929(4) 0.4395(2) 0.6271(3) 0.0320(13) Uani 1 1 d . . .
H45 H 0.9104 0.4484 0.5757 0.038 Uiso 1 1 calc R . .
C46 C 0.9161(4) 0.3881(2) 0.6579(3) 0.0348(14) Uani 1 1 d . . .
H46 H 0.9489 0.3611 0.628 0.042 Uiso 1 1 calc R . .
C47 C 0.8913(4) 0.3760(2) 0.7329(4) 0.0396(15) Uani 1 1 d . . .
H47 H 0.9068 0.3403 0.7547 0.047 Uiso 1 1 calc R . .
C48 C 0.8441(4) 0.41511(19) 0.7767(3) 0.0324(13) Uani 1 1 d . . .
H48 H 0.8292 0.4064 0.8289 0.039 Uiso 1 1 calc R . .
C49 C 0.6855(4) 0.47949(18) 0.8679(3) 0.0226(11) Uani 1 1 d . . .
C50 C 0.6846(4) 0.4937(2) 0.9473(3) 0.0287(12) Uani 1 1 d . . .
H50 H 0.7274 0.5235 0.9692 0.034 Uiso 1 1 calc R . .
C51 C 0.6216(5) 0.4643(2) 0.9945(4) 0.0425(15) Uani 1 1 d . . .
H51 H 0.622 0.4738 1.0488 0.051 Uiso 1 1 calc R . .
C52 C 0.5590(5) 0.4219(2) 0.9633(4) 0.0483(17) Uani 1 1 d . . .
H52 H 0.5156 0.402 0.9958 0.058 Uiso 1 1 calc R . .
C53 C 0.5586(4) 0.4078(2) 0.8852(4) 0.0371(15) Uani 1 1 d . . .
H53 H 0.5143 0.3783 0.8636 0.045 Uiso 1 1 calc R . .
C54 C 0.6212(4) 0.43576(19) 0.8380(3) 0.0300(13) Uani 1 1 d . . .
H54 H 0.6209 0.4252 0.7841 0.036 Uiso 1 1 calc R . .
N1 N 0.3627(3) 0.64020(15) 0.5981(2) 0.0241(10) Uani 1 1 d . . .
N2 N 0.3816(3) 0.69834(15) 0.6941(3) 0.0243(10) Uani 1 1 d . . .
O1 O 0.5198(2) 0.51868(12) 0.7381(2) 0.0234(8) Uani 1 1 d . . .
P1 P 0.75080(10) 0.65415(5) 0.71049(8) 0.0179(3) Uani 1 1 d . . .
P2 P 0.75841(10) 0.52159(5) 0.80126(8) 0.0191(3) Uani 1 1 d . . .
S1 S 0.42960(10) 0.52317(5) 0.79108(8) 0.0234(3) Uani 1 1 d . . .
Cl1 Cl 0.58512(9) 0.61515(5) 0.86439(7) 0.0232(3) Uani 1 1 d . . .
Cl2 Cl 0.63685(9) 0.55257(5) 0.60302(7) 0.0249(3) Uani 1 1 d . . .
Ge1 Ge 0.46033(4) 0.628649(19) 0.69683(3) 0.01897(14) Uani 1 1 d . . .
Ru1 Ru 0.63503(3) 0.586259(14) 0.73583(2) 0.01492(11) Uani 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 S1 1.797(5) . ?
C1 Ge1 2.050(5) . ?
C1 H1A 0.99 . ?
C1 H1B 0.99 . ?
C2 C7 1.364(7) . ?
C2 C3 1.366(7) . ?
C2 S1 1.794(5) . ?
C3 C4 1.375(7) . ?
C3 H3 0.95 . ?
C4 C5 1.366(9) . ?
C4 H4 0.95 . ?
C5 C6 1.364(10) . ?
C5 H5 0.95 . ?
C6 C7 1.375(8) . ?
C6 H6 0.95 . ?
C7 H7 0.95 . ?
C8 N2 1.333(6) . ?
C8 N1 1.338(6) . ?
C8 C15 1.524(7) . ?
C9 N1 1.499(6) . ?
C9 C11 1.513(7) . ?
C9 C10 1.540(7) . ?
C9 H9 1 . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 H11A 0.98 . ?
C11 H11B 0.98 . ?
C11 H11C 0.98 . ?
C12 N2 1.454(6) . ?
C12 C14 1.506(7) . ?
C12 C13 1.518(8) . ?
C12 H12 1 . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
C15 C16 1.507(7) . ?
C15 C17 1.542(7) . ?
C15 C18 1.542(7) . ?
C16 H16A 0.98 . ?
C16 H16B 0.98 . ?
C16 H16C 0.98 . ?
C17 H17A 0.98 . ?
C17 H17B 0.98 . ?
C17 H17C 0.98 . ?
C18 H18A 0.98 . ?
C18 H18B 0.98 . ?
C18 H18C 0.98 . ?
C19 C20 1.380(7) . ?
C19 C24 1.388(6) . ?
C19 P1 1.852(5) . ?
C20 C21 1.383(7) . ?
C20 H20 0.95 . ?
C21 C22 1.364(8) . ?
C21 H21 0.95 . ?
C22 C23 1.385(8) . ?
C22 H22 0.95 . ?
C23 C24 1.387(7) . ?
C23 H23 0.95 . ?
C24 H24 0.95 . ?
C25 C26 1.394(7) . ?
C25 C30 1.397(7) . ?
C25 P1 1.840(5) . ?
C26 C27 1.389(7) . ?
C26 H26 0.95 . ?
C27 C28 1.375(7) . ?
C27 H27 0.95 . ?
C28 C29 1.379(7) . ?
C28 H28 0.95 . ?
C29 C30 1.385(7) . ?
C29 H29 0.95 . ?
C30 H30 0.95 . ?
C31 C36 1.389(7) . ?
C31 C32 1.398(7) . ?
C31 P1 1.855(5) . ?
C32 C33 1.372(7) . ?
C32 H32 0.95 . ?
C33 C34 1.381(8) . ?
C33 H33 0.95 . ?
C34 C35 1.389(8) . ?
C34 H34 0.95 . ?
C35 C36 1.376(7) . ?
C35 H35 0.95 . ?
C36 H36 0.95 . ?
C37 C38 1.389(7) . ?
C37 C42 1.401(7) . ?
C37 P2 1.839(5) . ?
C38 C39 1.370(7) . ?
C38 H38 0.95 . ?
C39 C40 1.377(8) . ?
C39 H39 0.95 . ?
C40 C41 1.357(8) . ?
C40 H40 0.95 . ?
C41 C42 1.387(7) . ?
C41 H41 0.95 . ?
C42 H42 0.95 . ?
C43 C44 1.380(7) . ?
C43 C48 1.390(6) . ?
C43 P2 1.833(5) . ?
C44 C45 1.380(7) . ?
C44 H44 0.95 . ?
C45 C46 1.366(7) . ?
C45 H45 0.95 . ?
C46 C47 1.377(8) . ?
C46 H46 0.95 . ?
C47 C48 1.378(7) . ?
C47 H47 0.95 . ?
C48 H48 0.95 . ?
C49 C54 1.389(7) . ?
C49 C50 1.392(7) . ?
C49 P2 1.841(5) . ?
C50 C51 1.386(7) . ?
C50 H50 0.95 . ?
C51 C52 1.361(8) . ?
C51 H51 0.95 . ?
C52 C53 1.369(8) . ?
C52 H52 0.95 . ?
C53 C54 1.365(7) . ?
C53 H53 0.95 . ?
C54 H54 0.95 . ?
N1 Ge1 1.979(4) . ?
N2 Ge1 1.951(4) . ?
O1 S1 1.530(3) . ?
O1 Ru1 2.185(3) . ?
P1 Ru1 2.2661(12) . ?
P2 Ru1 2.3832(12) . ?
Cl1 Ru1 2.4410(12) . ?
Cl2 Ru1 2.3995(12) . ?
Ge1 Ru1 2.4429(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
S1 C1 Ge1 105.1(2) . . ?
S1 C1 H1A 110.7 . . ?
Ge1 C1 H1A 110.7 . . ?
S1 C1 H1B 110.7 . . ?
Ge1 C1 H1B 110.7 . . ?
H1A C1 H1B 108.8 . . ?
C7 C2 C3 121.1(5) . . ?
C7 C2 S1 118.4(4) . . ?
C3 C2 S1 120.4(4) . . ?
C2 C3 C4 118.7(6) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C5 C4 C3 119.9(6) . . ?
C5 C4 H4 120 . . ?
C3 C4 H4 120 . . ?
C6 C5 C4 121.4(6) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C5 C6 C7 118.5(6) . . ?
C5 C6 H6 120.8 . . ?
C7 C6 H6 120.8 . . ?
C2 C7 C6 120.3(6) . . ?
C2 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
N2 C8 N1 106.8(4) . . ?
N2 C8 C15 124.7(4) . . ?
N1 C8 C15 128.4(5) . . ?
N1 C9 C11 111.6(4) . . ?
N1 C9 C10 107.3(4) . . ?
C11 C9 C10 110.8(4) . . ?
N1 C9 H9 109 . . ?
C11 C9 H9 109 . . ?
C10 C9 H9 109 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 C14 109.9(4) . . ?
N2 C12 C13 109.4(4) . . ?
C14 C12 C13 111.0(5) . . ?
N2 C12 H12 108.8 . . ?
C14 C12 H12 108.8 . . ?
C13 C12 H12 108.8 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C8 115.5(4) . . ?
C16 C15 C17 106.1(4) . . ?
C8 C15 C17 108.5(4) . . ?
C16 C15 C18 106.8(5) . . ?
C8 C15 C18 108.2(4) . . ?
C17 C15 C18 111.9(4) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C24 117.5(5) . . ?
C20 C19 P1 119.6(4) . . ?
C24 C19 P1 122.9(4) . . ?
C19 C20 C21 121.2(5) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 H20 119.4 . . ?
C22 C21 C20 120.8(6) . . ?
C22 C21 H21 119.6 . . ?
C20 C21 H21 119.6 . . ?
C21 C22 C23 119.5(5) . . ?
C21 C22 H22 120.3 . . ?
C23 C22 H22 120.3 . . ?
C22 C23 C24 119.4(5) . . ?
C22 C23 H23 120.3 . . ?
C24 C23 H23 120.3 . . ?
C19 C24 C23 121.7(5) . . ?
C19 C24 H24 119.1 . . ?
C23 C24 H24 119.1 . . ?
C26 C25 C30 117.8(4) . . ?
C26 C25 P1 119.1(3) . . ?
C30 C25 P1 123.0(4) . . ?
C27 C26 C25 120.6(4) . . ?
C27 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
C28 C27 C26 120.8(5) . . ?
C28 C27 H27 119.6 . . ?
C26 C27 H27 119.6 . . ?
C27 C28 C29 119.3(5) . . ?
C27 C28 H28 120.3 . . ?
C29 C28 H28 120.3 . . ?
C28 C29 C30 120.3(5) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
C29 C30 C25 121.0(5) . . ?
C29 C30 H30 119.5 . . ?
C25 C30 H30 119.5 . . ?
C36 C31 C32 118.3(4) . . ?
C36 C31 P1 121.6(4) . . ?
C32 C31 P1 119.8(4) . . ?
C33 C32 C31 120.3(5) . . ?
C33 C32 H32 119.8 . . ?
C31 C32 H32 119.8 . . ?
C32 C33 C34 120.8(5) . . ?
C32 C33 H33 119.6 . . ?
C34 C33 H33 119.6 . . ?
C33 C34 C35 119.6(5) . . ?
C33 C34 H34 120.2 . . ?
C35 C34 H34 120.2 . . ?
C36 C35 C34 119.6(5) . . ?
C36 C35 H35 120.2 . . ?
C34 C35 H35 120.2 . . ?
C35 C36 C31 121.4(5) . . ?
C35 C36 H36 119.3 . . ?
C31 C36 H36 119.3 . . ?
C38 C37 C42 117.7(5) . . ?
C38 C37 P2 119.7(4) . . ?
C42 C37 P2 122.6(4) . . ?
C39 C38 C37 121.2(5) . . ?
C39 C38 H38 119.4 . . ?
C37 C38 H38 119.4 . . ?
C38 C39 C40 120.5(6) . . ?
C38 C39 H39 119.8 . . ?
C40 C39 H39 119.8 . . ?
C41 C40 C39 119.6(5) . . ?
C41 C40 H40 120.2 . . ?
C39 C40 H40 120.2 . . ?
C40 C41 C42 120.9(5) . . ?
C40 C41 H41 119.5 . . ?
C42 C41 H41 119.5 . . ?
C41 C42 C37 120.1(5) . . ?
C41 C42 H42 119.9 . . ?
C37 C42 H42 119.9 . . ?
C44 C43 C48 117.7(4) . . ?
C44 C43 P2 119.3(3) . . ?
C48 C43 P2 122.8(4) . . ?
C45 C44 C43 121.3(5) . . ?
C45 C44 H44 119.4 . . ?
C43 C44 H44 119.4 . . ?
C46 C45 C44 120.5(5) . . ?
C46 C45 H45 119.7 . . ?
C44 C45 H45 119.7 . . ?
C45 C46 C47 119.1(5) . . ?
C45 C46 H46 120.5 . . ?
C47 C46 H46 120.5 . . ?
C46 C47 C48 120.7(5) . . ?
C46 C47 H47 119.7 . . ?
C48 C47 H47 119.7 . . ?
C47 C48 C43 120.7(5) . . ?
C47 C48 H48 119.7 . . ?
C43 C48 H48 119.7 . . ?
C54 C49 C50 118.1(5) . . ?
C54 C49 P2 120.4(4) . . ?
C50 C49 P2 121.2(4) . . ?
C51 C50 C49 120.2(5) . . ?
C51 C50 H50 119.9 . . ?
C49 C50 H50 119.9 . . ?
C52 C51 C50 120.2(6) . . ?
C52 C51 H51 119.9 . . ?
C50 C51 H51 119.9 . . ?
C51 C52 C53 120.1(5) . . ?
C51 C52 H52 119.9 . . ?
C53 C52 H52 119.9 . . ?
C54 C53 C52 120.4(5) . . ?
C54 C53 H53 119.8 . . ?
C52 C53 H53 119.8 . . ?
C53 C54 C49 120.9(6) . . ?
C53 C54 H54 119.5 . . ?
C49 C54 H54 119.5 . . ?
C8 N1 C9 134.5(4) . . ?
C8 N1 Ge1 92.8(3) . . ?
C9 N1 Ge1 132.1(3) . . ?
C8 N2 C12 132.1(4) . . ?
C8 N2 Ge1 94.2(3) . . ?
C12 N2 Ge1 133.5(3) . . ?
S1 O1 Ru1 119.64(17) . . ?
C25 P1 C19 99.8(2) . . ?
C25 P1 C31 101.5(2) . . ?
C19 P1 C31 101.3(2) . . ?
C25 P1 Ru1 122.47(16) . . ?
C19 P1 Ru1 116.37(16) . . ?
C31 P1 Ru1 112.36(14) . . ?
C43 P2 C37 102.3(2) . . ?
C43 P2 C49 100.6(2) . . ?
C37 P2 C49 101.9(2) . . ?
C43 P2 Ru1 120.78(17) . . ?
C37 P2 Ru1 120.23(15) . . ?
C49 P2 Ru1 107.80(15) . . ?
O1 S1 C2 101.9(2) . . ?
O1 S1 C1 105.0(2) . . ?
C2 S1 C1 101.9(2) . . ?
N2 Ge1 N1 66.13(16) . . ?
N2 Ge1 C1 96.38(17) . . ?
N1 Ge1 C1 97.96(19) . . ?
N2 Ge1 Ru1 143.65(12) . . ?
N1 Ge1 Ru1 137.58(11) . . ?
C1 Ge1 Ru1 104.16(13) . . ?
O1 Ru1 P1 170.10(9) . . ?
O1 Ru1 P2 84.15(9) . . ?
P1 Ru1 P2 99.56(4) . . ?
O1 Ru1 Cl2 80.86(9) . . ?
P1 Ru1 Cl2 89.50(4) . . ?
P2 Ru1 Cl2 98.00(4) . . ?
O1 Ru1 Cl1 87.65(9) . . ?
P1 Ru1 Cl1 101.50(4) . . ?
P2 Ru1 Cl1 89.49(4) . . ?
Cl2 Ru1 Cl1 165.53(4) . . ?
O1 Ru1 Ge1 75.06(8) . . ?
P1 Ru1 Ge1 102.77(3) . . ?
P2 Ru1 Ge1 156.45(4) . . ?
Cl2 Ru1 Ge1 89.61(3) . . ?
Cl1 Ru1 Ge1 78.87(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_NL-154
_database_code_depnum_ccdc_archive 'CCDC 1855504'
_audit_update_record             
;
2018-07-12 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C42 H64 Ge2 N4 O6 S2 W, 2(C4 H8 O)'
_chemical_formula_sum            'C50 H80 Ge2 N4 O8 S2 W'
_chemical_formula_weight         1258.36
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.9512(4)
_cell_length_b                   11.6654(5)
_cell_length_c                   13.3526(6)
_cell_angle_alpha                79.8470(10)
_cell_angle_beta                 77.244(2)
_cell_angle_gamma                70.587(2)
_cell_volume                     1416.88(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    9891
_cell_measurement_theta_min      3.15
_cell_measurement_theta_max      31.88
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             642
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.203
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_absorpt_correction_T_min  0.6343
_exptl_absorpt_correction_T_max  0.7463

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine focus sealed tube'
_diffrn_radiation_monochromator  triumph
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_number            36625
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.15
_diffrn_reflns_theta_max         31.91
_diffrn_reflns_theta_full        31.91
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_reflns_number_total             9692
_reflns_number_gt                8473
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       APEX2
_computing_cell_refinement       'APEX2 and SAINT'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0104P)²+1.2203P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         9692
_refine_ls_number_parameters     332
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0301
_refine_ls_wR_factor_ref         0.0576
_refine_ls_wR_factor_gt          0.0544
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.114
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.103

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.849 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1143(2) 0.72316(18) 0.33047(16) 0.0213(4) Uani 1 1 d . . .
C2 C 0.3596(2) 0.5307(2) 0.63484(18) 0.0272(4) Uani 1 1 d . B .
C3 C 0.4071(2) 0.3784(2) 0.47871(17) 0.0275(5) Uani 1 1 d . B .
C5 C -0.0253(2) 0.7585(2) 0.28587(18) 0.0274(5) Uani 1 1 d . . .
C6 C -0.1535(3) 0.8509(2) 0.3445(2) 0.0357(5) Uani 1 1 d . . .
H6A H -0.1775 0.8147 0.4155 0.054 Uiso 1 1 calc R . .
H6B H -0.2373 0.8722 0.31 0.054 Uiso 1 1 calc R . .
H6C H -0.1278 0.9247 0.3455 0.054 Uiso 1 1 calc R . .
C7 C -0.0672(3) 0.6421(2) 0.2889(2) 0.0407(6) Uani 1 1 d . . .
H7A H -0.0812 0.604 0.3604 0.061 Uiso 1 1 calc R . .
H7B H 0.0101 0.5845 0.2466 0.061 Uiso 1 1 calc R . .
H7C H -0.1573 0.6636 0.2617 0.061 Uiso 1 1 calc R . .
C8 C 0.0008(3) 0.8203(3) 0.1746(2) 0.0437(7) Uani 1 1 d . . .
H8A H -0.0906 0.8517 0.1482 0.066 Uiso 1 1 calc R . .
H8B H 0.0711 0.7604 0.1307 0.066 Uiso 1 1 calc R . .
H8C H 0.0385 0.8881 0.1741 0.066 Uiso 1 1 calc R . .
C9 C 0.0365(2) 0.8028(2) 0.50868(18) 0.0285(5) Uani 1 1 d . . .
H9 H -0.0459 0.8734 0.4877 0.034 Uiso 1 1 calc R . .
C10 C -0.0231(3) 0.7047(3) 0.5748(2) 0.0440(7) Uani 1 1 d . . .
H10A H -0.0733 0.6753 0.5342 0.066 Uiso 1 1 calc R . .
H10B H -0.0912 0.739 0.6352 0.066 Uiso 1 1 calc R . .
H10C H 0.0567 0.6364 0.5978 0.066 Uiso 1 1 calc R . .
C11 C 0.1200(3) 0.8476(2) 0.5681(2) 0.0393(6) Uani 1 1 d . . .
H11A H 0.2004 0.7787 0.5896 0.059 Uiso 1 1 calc R . .
H11B H 0.0553 0.8827 0.6293 0.059 Uiso 1 1 calc R . .
H11C H 0.1582 0.9101 0.5236 0.059 Uiso 1 1 calc R . .
C12 C 0.2901(3) 0.5938(2) 0.19245(18) 0.0300(5) Uani 1 1 d . . .
H12 H 0.2035 0.6059 0.1608 0.036 Uiso 1 1 calc R . .
C13 C 0.3589(4) 0.4580(3) 0.2201(2) 0.0480(7) Uani 1 1 d . . .
H13A H 0.4432 0.4453 0.2521 0.072 Uiso 1 1 calc R . .
H13B H 0.3896 0.4165 0.1574 0.072 Uiso 1 1 calc R . .
H13C H 0.2884 0.4244 0.2688 0.072 Uiso 1 1 calc R . .
C14 C 0.3952(4) 0.6491(3) 0.1161(2) 0.0547(8) Uani 1 1 d . . .
H14A H 0.3494 0.7373 0.1015 0.082 Uiso 1 1 calc R . .
H14B H 0.4222 0.6109 0.0518 0.082 Uiso 1 1 calc R . .
H14C H 0.4821 0.635 0.1455 0.082 Uiso 1 1 calc R . .
C16 C 0.4638(3) 1.0939(2) 0.2948(2) 0.0422(6) Uani 1 1 d . B .
H16 H 0.4039 1.1053 0.3606 0.051 Uiso 1 1 calc R . .
C17 C 0.5720(3) 1.1491(2) 0.2619(2) 0.0417(6) Uani 1 1 d . . .
H17 H 0.5863 1.1979 0.3061 0.05 Uiso 1 1 calc R . .
C18 C 0.6592(3) 1.1347(2) 0.1665(2) 0.0385(6) Uani 1 1 d . . .
C19 C 0.6367(3) 1.0639(3) 0.1027(2) 0.0445(7) Uani 1 1 d . . .
H19 H 0.6954 1.0539 0.0363 0.053 Uiso 1 1 calc R . .
C20 C 0.5294(4) 1.0072(3) 0.1345(2) 0.0465(7) Uani 1 1 d . B .
H20 H 0.5147 0.9586 0.0902 0.056 Uiso 1 1 calc R . .
C21 C 0.7783(4) 1.1933(3) 0.1330(3) 0.0586(9) Uani 1 1 d . . .
H21A H 0.8477 1.1613 0.1807 0.088 Uiso 1 1 calc R . .
H21B H 0.7368 1.2821 0.1336 0.088 Uiso 1 1 calc R . .
H21C H 0.8278 1.1748 0.063 0.088 Uiso 1 1 calc R . .
C22 C 0.1015(6) 0.3288(5) 0.1317(3) 0.0980(16) Uani 1 1 d . . .
H22A H -0.0016 0.3406 0.1622 0.118 Uiso 1 1 calc R . .
H22B H 0.1594 0.2934 0.1875 0.118 Uiso 1 1 calc R . .
C23 C 0.1457(5) 0.2471(5) 0.0539(4) 0.0903(14) Uani 1 1 d . . .
H23A H 0.0643 0.2534 0.0199 0.108 Uiso 1 1 calc R . .
H23B H 0.1862 0.1612 0.0831 0.108 Uiso 1 1 calc R . .
C24 C 0.2591(5) 0.2923(4) -0.0192(4) 0.0819(13) Uani 1 1 d . . .
H24A H 0.3551 0.2533 0.0015 0.098 Uiso 1 1 calc R . .
H24B H 0.2652 0.276 -0.0906 0.098 Uiso 1 1 calc R . .
C25 C 0.2084(4) 0.4252(4) -0.0106(3) 0.0722(11) Uani 1 1 d . . .
H25A H 0.2921 0.4559 -0.0182 0.087 Uiso 1 1 calc R . .
H25B H 0.1518 0.4697 -0.0656 0.087 Uiso 1 1 calc R . .
N1 N 0.13459(19) 0.75644(16) 0.41603(14) 0.0231(4) Uani 1 1 d . . .
N2 N 0.24359(19) 0.65513(17) 0.28631(14) 0.0237(4) Uani 1 1 d . . .
O2 O 0.2826(2) 0.5454(2) 0.71229(15) 0.0458(5) Uani 1 1 d . . .
O3 O 0.3561(2) 0.30738(19) 0.46808(15) 0.0471(5) Uani 1 1 d . . .
O4 O 0.1215(3) 0.4437(3) 0.0872(2) 0.0735(8) Uani 1 1 d . . .
C4 C 0.4229(2) 0.8064(2) 0.32867(19) 0.0288(5) Uani 1 1 d D . .
H4A H 0.4721 0.822 0.3794 0.035 Uiso 1 1 calc R A 1
H4B H 0.4985 0.7768 0.269 0.035 Uiso 1 1 calc R A 1
C15 C 0.4442(3) 1.0221(2) 0.2310(2) 0.0380(6) Uani 1 1 d D . .
S1 S 0.3030(6) 0.9510(5) 0.2842(4) 0.0386(8) Uani 0.584(5) 1 d PDU B 1
O1 O 0.2512(4) 0.9369(3) 0.1926(3) 0.0545(12) Uani 0.584(5) 1 d PDU B 1
S1' S 0.3170(9) 0.9362(7) 0.2592(6) 0.0435(14) Uani 0.416(5) 1 d PDU B 2
O1' O 0.2007(5) 1.0073(4) 0.3336(5) 0.067(2) Uani 0.416(5) 1 d PDU B 2
Ge1 Ge 0.34158(2) 0.669758(18) 0.393583(16) 0.01977(5) Uani 1 1 d . B .
W1 W 0.5 0.5 0.5 0.02041(3) Uani 1 2 d S . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 N2 1.335(3) . ?
C1 N1 1.344(3) . ?
C1 C5 1.534(3) . ?
C2 O2 1.145(3) . ?
C2 W1 2.026(2) . ?
C3 O3 1.147(3) . ?
C3 W1 2.020(2) . ?
C5 C6 1.531(3) . ?
C5 C8 1.539(3) . ?
C5 C7 1.540(3) . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
C8 H8A 0.98 . ?
C8 H8B 0.98 . ?
C8 H8C 0.98 . ?
C9 N1 1.459(3) . ?
C9 C10 1.518(3) . ?
C9 C11 1.523(3) . ?
C9 H9 1 . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 H11A 0.98 . ?
C11 H11B 0.98 . ?
C11 H11C 0.98 . ?
C12 N2 1.462(3) . ?
C12 C14 1.515(4) . ?
C12 C13 1.517(4) . ?
C12 H12 1 . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
C16 C15 1.377(4) . ?
C16 C17 1.385(4) . ?
C16 H16 0.95 . ?
C17 C18 1.377(4) . ?
C17 H17 0.95 . ?
C18 C19 1.383(4) . ?
C18 C21 1.506(4) . ?
C19 C20 1.389(4) . ?
C19 H19 0.95 . ?
C20 C15 1.382(4) . ?
C20 H20 0.95 . ?
C21 H21A 0.98 . ?
C21 H21B 0.98 . ?
C21 H21C 0.98 . ?
C22 O4 1.426(5) . ?
C22 C23 1.432(6) . ?
C22 H22A 0.99 . ?
C22 H22B 0.99 . ?
C23 C24 1.494(5) . ?
C23 H23A 0.99 . ?
C23 H23B 0.99 . ?
C24 C25 1.480(6) . ?
C24 H24A 0.99 . ?
C24 H24B 0.99 . ?
C25 O4 1.406(4) . ?
C25 H25A 0.99 . ?
C25 H25B 0.99 . ?
N1 Ge1 1.9506(18) . ?
N2 Ge1 1.9609(17) . ?
C4 S1' 1.772(8) . ?
C4 S1 1.801(6) . ?
C4 Ge1 2.002(2) . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
C15 S1' 1.803(9) . ?
C15 S1 1.815(6) . ?
S1 O1 1.481(6) . ?
S1' O1' 1.470(8) . ?
Ge1 W1 2.5195(2) . ?
W1 C3 2.019(2) 2_666 ?
W1 C2 2.026(2) 2_666 ?
W1 Ge1 2.5195(2) 2_666 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 C1 N1 106.56(17) . . ?
N2 C1 C5 124.78(19) . . ?
N1 C1 C5 128.60(19) . . ?
O2 C2 W1 178.2(2) . . ?
O3 C3 W1 178.4(2) . . ?
C6 C5 C1 113.87(19) . . ?
C6 C5 C8 106.0(2) . . ?
C1 C5 C8 108.85(19) . . ?
C6 C5 C7 108.2(2) . . ?
C1 C5 C7 108.59(19) . . ?
C8 C5 C7 111.4(2) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 C10 111.2(2) . . ?
N1 C9 C11 107.75(19) . . ?
C10 C9 C11 111.0(2) . . ?
N1 C9 H9 109 . . ?
C10 C9 H9 109 . . ?
C11 C9 H9 109 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 C14 109.6(2) . . ?
N2 C12 C13 109.3(2) . . ?
C14 C12 C13 111.2(2) . . ?
N2 C12 H12 108.9 . . ?
C14 C12 H12 108.9 . . ?
C13 C12 H12 108.9 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C15 C16 C17 119.2(3) . . ?
C15 C16 H16 120.4 . . ?
C17 C16 H16 120.4 . . ?
C18 C17 C16 121.4(3) . . ?
C18 C17 H17 119.3 . . ?
C16 C17 H17 119.3 . . ?
C17 C18 C19 118.7(2) . . ?
C17 C18 C21 120.6(3) . . ?
C19 C18 C21 120.7(3) . . ?
C18 C19 C20 120.8(3) . . ?
C18 C19 H19 119.6 . . ?
C20 C19 H19 119.6 . . ?
C15 C20 C19 119.4(3) . . ?
C15 C20 H20 120.3 . . ?
C19 C20 H20 120.3 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O4 C22 C23 109.7(3) . . ?
O4 C22 H22A 109.7 . . ?
C23 C22 H22A 109.7 . . ?
O4 C22 H22B 109.7 . . ?
C23 C22 H22B 109.7 . . ?
H22A C22 H22B 108.2 . . ?
C22 C23 C24 101.9(4) . . ?
C22 C23 H23A 111.4 . . ?
C24 C23 H23A 111.4 . . ?
C22 C23 H23B 111.4 . . ?
C24 C23 H23B 111.4 . . ?
H23A C23 H23B 109.3 . . ?
C25 C24 C23 103.4(3) . . ?
C25 C24 H24A 111.1 . . ?
C23 C24 H24A 111.1 . . ?
C25 C24 H24B 111.1 . . ?
C23 C24 H24B 111.1 . . ?
H24A C24 H24B 109.1 . . ?
O4 C25 C24 107.7(3) . . ?
O4 C25 H25A 110.2 . . ?
C24 C25 H25A 110.2 . . ?
O4 C25 H25B 110.2 . . ?
C24 C25 H25B 110.2 . . ?
H25A C25 H25B 108.5 . . ?
C1 N1 C9 133.08(18) . . ?
C1 N1 Ge1 93.51(13) . . ?
C9 N1 Ge1 130.62(14) . . ?
C1 N2 C12 132.06(18) . . ?
C1 N2 Ge1 93.32(13) . . ?
C12 N2 Ge1 134.62(15) . . ?
C25 O4 C22 106.6(3) . . ?
S1' C4 Ge1 119.7(3) . . ?
S1 C4 Ge1 119.2(2) . . ?
S1' C4 H4A 116.9 . . ?
S1 C4 H4A 107.5 . . ?
Ge1 C4 H4A 107.5 . . ?
S1' C4 H4B 96.6 . . ?
S1 C4 H4B 107.5 . . ?
Ge1 C4 H4B 107.5 . . ?
H4A C4 H4B 107 . . ?
C16 C15 C20 120.5(2) . . ?
C16 C15 S1' 127.1(3) . . ?
C20 C15 S1' 112.3(3) . . ?
C16 C15 S1 115.1(3) . . ?
C20 C15 S1 124.4(3) . . ?
O1 S1 C4 109.4(4) . . ?
O1 S1 C15 104.4(3) . . ?
C4 S1 C15 95.4(3) . . ?
O1' S1' C4 108.3(5) . . ?
O1' S1' C15 102.0(5) . . ?
C4 S1' C15 96.9(4) . . ?
N1 Ge1 N2 66.61(7) . . ?
N1 Ge1 C4 101.18(8) . . ?
N2 Ge1 C4 102.18(9) . . ?
N1 Ge1 W1 132.68(5) . . ?
N2 Ge1 W1 127.82(5) . . ?
C4 Ge1 W1 115.30(6) . . ?
C3 W1 C3 180.0000(10) 2_666 . ?
C3 W1 C2 91.01(9) 2_666 . ?
C3 W1 C2 88.99(9) . . ?
C3 W1 C2 88.99(9) 2_666 2_666 ?
C3 W1 C2 91.01(9) . 2_666 ?
C2 W1 C2 180 . 2_666 ?
C3 W1 Ge1 88.12(7) 2_666 . ?
C3 W1 Ge1 91.88(7) . . ?
C2 W1 Ge1 94.54(6) . . ?
C2 W1 Ge1 85.46(6) 2_666 . ?
C3 W1 Ge1 91.88(7) 2_666 2_666 ?
C3 W1 Ge1 88.12(7) . 2_666 ?
C2 W1 Ge1 85.46(6) . 2_666 ?
C2 W1 Ge1 94.54(6) 2_666 2_666 ?
Ge1 W1 Ge1 179.999(9) . 2_666 ?

####################################################################### 
# 
# 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_NL-336
_database_code_depnum_ccdc_archive 'CCDC 1855505'
_audit_update_record             
;
2018-07-12 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C42 H64 Ge2 Mo N4 O6 S2, 2(C4 H8 O)'
_chemical_formula_sum            'C50 H80 Ge2 Mo N4 O8 S2'
_chemical_formula_weight         1170.46

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.9669(5)
_cell_length_b                   11.7085(8)
_cell_length_c                   13.3702(10)
_cell_angle_alpha                79.929(3)
_cell_angle_beta                 77.221(2)
_cell_angle_gamma                70.656(2)
_cell_volume                     1426.94(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    5856
_cell_measurement_theta_min      3.18
_cell_measurement_theta_max      25.68

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             610
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_absorpt_correction_T_min  0.6702
_exptl_absorpt_correction_T_max  0.7453

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine focus sealed tube'
_diffrn_radiation_monochromator  triumph
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_unetI/netI     0.0684
_diffrn_reflns_number            21442
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.144
_diffrn_reflns_theta_max         25.684
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.978
_reflns_Friedel_coverage         0
_reflns_number_total             5306
_reflns_number_gt                3889
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       APEX2
_computing_cell_refinement       SAINT
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'


#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0001P)²+4.1846P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5306
_refine_ls_number_parameters     332
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0658
_refine_ls_wR_factor_ref         0.0939
_refine_ls_wR_factor_gt          0.0867
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.12
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.115

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.6397(5) 0.4701(4) 0.3648(4) 0.0295(11) Uani 1 1 d . . . . .
C2 C 0.4066(5) 0.3784(4) 0.4785(3) 0.0291(11) Uani 1 1 d . . . . .
C3 C 0.8856(5) 0.2765(4) 0.6697(3) 0.0233(10) Uani 1 1 d . . . . .
C4 C 1.0247(5) 0.2410(4) 0.7144(4) 0.0299(11) Uani 1 1 d . . . . .
C5 C 1.1531(5) 0.1490(4) 0.6557(4) 0.0386(12) Uani 1 1 d . . . . .
H5A H 1.1263 0.0766 0.6524 0.058 Uiso 1 1 calc R U . . .
H5B H 1.2356 0.1257 0.6915 0.058 Uiso 1 1 calc R U . . .
H5C H 1.1794 0.1861 0.5855 0.058 Uiso 1 1 calc R U . . .
C6 C 1.0668(6) 0.3572(5) 0.7119(4) 0.0435(14) Uani 1 1 d . . . . .
H6A H 1.0828 0.3944 0.6405 0.065 Uiso 1 1 calc R U . . .
H6B H 1.1555 0.3359 0.7405 0.065 Uiso 1 1 calc R U . . .
H6C H 0.9887 0.415 0.7532 0.065 Uiso 1 1 calc R U . . .
C7 C 0.9990(6) 0.1788(5) 0.8255(4) 0.0462(14) Uani 1 1 d . . . . .
H7A H 0.9301 0.2385 0.87 0.069 Uiso 1 1 calc R U . . .
H7B H 1.0906 0.1463 0.8512 0.069 Uiso 1 1 calc R U . . .
H7C H 0.9598 0.1122 0.8258 0.069 Uiso 1 1 calc R U . . .
C8 C 0.9631(5) 0.1973(4) 0.4912(3) 0.0299(11) Uani 1 1 d . . . . .
H8 H 1.0455 0.1273 0.512 0.036 Uiso 1 1 calc R U . . .
C9 C 1.0230(6) 0.2953(5) 0.4249(4) 0.0470(14) Uani 1 1 d . . . . .
H9A H 0.944 0.3617 0.3994 0.071 Uiso 1 1 calc R U . . .
H9B H 1.0941 0.2602 0.3662 0.071 Uiso 1 1 calc R U . . .
H9C H 1.0695 0.3271 0.4663 0.071 Uiso 1 1 calc R U . . .
C10 C 0.8804(6) 0.1520(5) 0.4319(4) 0.0417(13) Uani 1 1 d . . . . .
H10A H 0.8395 0.0918 0.4771 0.063 Uiso 1 1 calc R U . . .
H10B H 0.9462 0.1142 0.3723 0.063 Uiso 1 1 calc R U . . .
H10C H 0.8023 0.2207 0.408 0.063 Uiso 1 1 calc R U . . .
C11 C 0.7095(5) 0.4056(4) 0.8079(3) 0.0311(11) Uani 1 1 d . . . . .
H11 H 0.796 0.3929 0.8397 0.037 Uiso 1 1 calc R U . . .
C12 C 0.6426(6) 0.5410(5) 0.7808(4) 0.0486(15) Uani 1 1 d . . . . .
H12A H 0.7143 0.5742 0.7334 0.073 Uiso 1 1 calc R U . . .
H12B H 0.6107 0.5818 0.8438 0.073 Uiso 1 1 calc R U . . .
H12C H 0.5595 0.5546 0.7475 0.073 Uiso 1 1 calc R U . . .
C13 C 0.6040(6) 0.3509(6) 0.8844(4) 0.0561(16) Uani 1 1 d . . . . .
H13A H 0.517 0.3657 0.8552 0.084 Uiso 1 1 calc R U . . .
H13B H 0.5777 0.3888 0.9487 0.084 Uiso 1 1 calc R U . . .
H13C H 0.6491 0.263 0.8986 0.084 Uiso 1 1 calc R U . . .
C14 C 0.5770(5) 0.1940(4) 0.6709(4) 0.0301(11) Uani 1 1 d D . . . .
H14A H 0.5012 0.2236 0.7304 0.036 Uiso 1 1 calc R U . A 1
H14B H 0.5285 0.1782 0.6201 0.036 Uiso 1 1 calc R U . A 1
C15 C 0.5554(6) -0.0215(4) 0.7693(4) 0.0388(13) Uani 1 1 d D . . . .
S1 S 0.6962(9) 0.0503(8) 0.7157(10) 0.041(2) Uani 0.572(9) 1 d D U P B 1
O3 O 0.7475(8) 0.0644(6) 0.8077(6) 0.057(3) Uani 0.572(9) 1 d D U P B 1
S1' S 0.6835(12) 0.0634(11) 0.7405(13) 0.046(4) Uani 0.428(9) 1 d D U P B 2
O3' O 0.7999(10) -0.0073(8) 0.6649(9) 0.075(4) Uani 0.428(9) 1 d D U P B 2
C16 C 0.4703(7) -0.0072(5) 0.8657(4) 0.0484(15) Uani 1 1 d . . . . .
H16 H 0.4849 0.0413 0.9099 0.058 Uiso 1 1 calc R U . . .
C17 C 0.3637(6) -0.0635(5) 0.8976(4) 0.0462(14) Uani 1 1 d . . . . .
H17 H 0.3055 -0.0538 0.9641 0.055 Uiso 1 1 calc R U . . .
C18 C 0.3408(6) -0.1341(4) 0.8336(4) 0.0403(13) Uani 1 1 d . . . . .
C19 C 0.4292(6) -0.1487(5) 0.7386(4) 0.0444(14) Uani 1 1 d . . . . .
H19 H 0.4159 -0.1982 0.6945 0.053 Uiso 1 1 calc R U . . .
C20 C 0.5363(6) -0.0934(5) 0.7058(4) 0.0441(13) Uani 1 1 d . . . . .
H20 H 0.5963 -0.1048 0.64 0.053 Uiso 1 1 calc R U . . .
C21 C 0.2236(7) -0.1941(6) 0.8668(5) 0.0610(18) Uani 1 1 d . . . . .
H21A H 0.1431 -0.1499 0.8302 0.092 Uiso 1 1 calc R U . . .
H21B H 0.1895 -0.1929 0.9413 0.092 Uiso 1 1 calc R U . . .
H21C H 0.2618 -0.2786 0.8505 0.092 Uiso 1 1 calc R U . . .
C22 C 0.9005(12) 0.6721(10) 0.8691(7) 0.121(4) Uani 1 1 d . . . . .
H22A H 0.8464 0.7065 0.8113 0.146 Uiso 1 1 calc R U . . .
H22B H 1.0043 0.6599 0.8414 0.146 Uiso 1 1 calc R U . . .
C23 C 0.8519(10) 0.7558(8) 0.9459(7) 0.102(3) Uani 1 1 d . . . . .
H23A H 0.8104 0.8404 0.9156 0.122 Uiso 1 1 calc R U . . .
H23B H 0.9313 0.752 0.9809 0.122 Uiso 1 1 calc R U . . .
C24 C 0.7409(9) 0.7103(8) 1.0168(7) 0.095(3) Uani 1 1 d . . . . .
H24A H 0.6458 0.7479 0.9949 0.113 Uiso 1 1 calc R U . . .
H24B H 0.7325 0.7283 1.088 0.113 Uiso 1 1 calc R U . . .
C25 C 0.7919(8) 0.5756(8) 1.0111(6) 0.083(2) Uani 1 1 d . . . . .
H25A H 0.8487 0.5328 1.0661 0.099 Uiso 1 1 calc R U . . .
H25B H 0.7087 0.5444 1.0193 0.099 Uiso 1 1 calc R U . . .
Mo1 Mo 0.5 0.5 0.5 0.02002(14) Uani 1 2 d S . P . .
Ge1 Ge 0.65859(5) 0.33051(4) 0.60618(4) 0.02178(13) Uani 1 1 d . . . . .
N1 N 0.8654(4) 0.2434(3) 0.5843(3) 0.0252(8) Uani 1 1 d . . . . .
N2 N 0.7563(4) 0.3440(3) 0.7141(3) 0.0248(8) Uani 1 1 d . . . . .
O1 O 0.7169(4) 0.4554(4) 0.2871(3) 0.0475(10) Uani 1 1 d . . . . .
O2 O 0.3564(4) 0.3074(4) 0.4679(3) 0.0499(10) Uani 1 1 d . . . . .
O4 O 0.8787(6) 0.5576(5) 0.9128(4) 0.0867(16) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.150(6) . ?
C1 Mo1 2.028(5) . ?
C2 O2 1.144(5) . ?
C2 Mo1 2.029(5) . ?
C3 N2 1.338(5) . ?
C3 N1 1.343(5) . ?
C3 C4 1.533(6) . ?
C4 C5 1.533(7) . ?
C4 C7 1.543(7) . ?
C4 C6 1.545(6) . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
C8 N1 1.463(6) . ?
C8 C10 1.522(6) . ?
C8 C9 1.524(7) . ?
C8 H8 1 . ?
C9 H9A 0.98 . ?
C9 H9B 0.98 . ?
C9 H9C 0.98 . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 N2 1.465(6) . ?
C11 C12 1.515(7) . ?
C11 C13 1.517(7) . ?
C11 H11 1 . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C14 S1' 1.787(11) . ?
C14 S1 1.799(9) . ?
C14 Ge1 2.008(4) . ?
C14 H14A 0.99 . ?
C14 H14B 0.99 . ?
C15 C20 1.377(7) . ?
C15 C16 1.380(8) . ?
C15 S1' 1.804(12) . ?
C15 S1 1.821(9) . ?
S1 O3 1.485(13) . ?
S1' O3' 1.480(17) . ?
C16 C17 1.382(7) . ?
C16 H16 0.95 . ?
C17 C18 1.388(7) . ?
C17 H17 0.95 . ?
C18 C19 1.378(7) . ?
C18 C21 1.504(7) . ?
C19 C20 1.380(7) . ?
C19 H19 0.95 . ?
C20 H20 0.95 . ?
C21 H21A 0.98 . ?
C21 H21B 0.98 . ?
C21 H21C 0.98 . ?
C22 O4 1.431(10) . ?
C22 C23 1.438(11) . ?
C22 H22A 0.99 . ?
C22 H22B 0.99 . ?
C23 C24 1.468(10) . ?
C23 H23A 0.99 . ?
C23 H23B 0.99 . ?
C24 C25 1.498(10) . ?
C24 H24A 0.99 . ?
C24 H24B 0.99 . ?
C25 O4 1.412(8) . ?
C25 H25A 0.99 . ?
C25 H25B 0.99 . ?
Mo1 C1 2.028(5) 2_666 ?
Mo1 C2 2.029(5) 2_666 ?
Mo1 Ge1 2.5261(4) . ?
Mo1 Ge1 2.5261(5) 2_666 ?
Ge1 N1 1.955(4) . ?
Ge1 N2 1.964(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
O1 C1 Mo1 178.4(4) . . ?
O2 C2 Mo1 178.2(4) . . ?
N2 C3 N1 106.5(4) . . ?
N2 C3 C4 124.8(4) . . ?
N1 C3 C4 128.6(4) . . ?
C3 C4 C5 114.0(4) . . ?
C3 C4 C7 109.1(4) . . ?
C5 C4 C7 105.8(4) . . ?
C3 C4 C6 108.5(4) . . ?
C5 C4 C6 108.2(4) . . ?
C7 C4 C6 111.3(4) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C10 108.2(4) . . ?
N1 C8 C9 111.3(4) . . ?
C10 C8 C9 111.1(4) . . ?
N1 C8 H8 108.7 . . ?
C10 C8 H8 108.7 . . ?
C9 C8 H8 108.7 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 C12 109.7(4) . . ?
N2 C11 C13 109.7(4) . . ?
C12 C11 C13 111.4(4) . . ?
N2 C11 H11 108.7 . . ?
C12 C11 H11 108.7 . . ?
C13 C11 H11 108.7 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
S1' C14 Ge1 119.8(4) . . ?
S1 C14 Ge1 119.2(3) . . ?
S1 C14 H14A 107.5 . . ?
Ge1 C14 H14A 107.5 . . ?
S1 C14 H14B 107.5 . . ?
Ge1 C14 H14B 107.5 . . ?
H14A C14 H14B 107 . . ?
C20 C15 C16 120.3(5) . . ?
C20 C15 S1' 126.7(7) . . ?
C16 C15 S1' 113.0(7) . . ?
C20 C15 S1 115.1(6) . . ?
C16 C15 S1 124.7(6) . . ?
O3 S1 C14 109.5(7) . . ?
O3 S1 C15 104.0(7) . . ?
C14 S1 C15 95.8(4) . . ?
O3' S1' C14 107.9(10) . . ?
O3' S1' C15 102.5(10) . . ?
C14 S1' C15 96.8(6) . . ?
C15 C16 C17 119.8(5) . . ?
C15 C16 H16 120.1 . . ?
C17 C16 H16 120.1 . . ?
C16 C17 C18 120.7(5) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 H17 119.7 . . ?
C19 C18 C17 118.3(5) . . ?
C19 C18 C21 120.5(5) . . ?
C17 C18 C21 121.2(5) . . ?
C18 C19 C20 121.6(5) . . ?
C18 C19 H19 119.2 . . ?
C20 C19 H19 119.2 . . ?
C15 C20 C19 119.3(5) . . ?
C15 C20 H20 120.4 . . ?
C19 C20 H20 120.4 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O4 C22 C23 110.4(7) . . ?
O4 C22 H22A 109.6 . . ?
C23 C22 H22A 109.6 . . ?
O4 C22 H22B 109.6 . . ?
C23 C22 H22B 109.6 . . ?
H22A C22 H22B 108.1 . . ?
C22 C23 C24 101.7(7) . . ?
C22 C23 H23A 111.4 . . ?
C24 C23 H23A 111.4 . . ?
C22 C23 H23B 111.4 . . ?
C24 C23 H23B 111.4 . . ?
H23A C23 H23B 109.3 . . ?
C23 C24 C25 104.9(7) . . ?
C23 C24 H24A 110.8 . . ?
C25 C24 H24A 110.8 . . ?
C23 C24 H24B 110.8 . . ?
C25 C24 H24B 110.8 . . ?
H24A C24 H24B 108.8 . . ?
O4 C25 C24 106.1(6) . . ?
O4 C25 H25A 110.5 . . ?
C24 C25 H25A 110.5 . . ?
O4 C25 H25B 110.5 . . ?
C24 C25 H25B 110.5 . . ?
H25A C25 H25B 108.7 . . ?
C1 Mo1 C1 180.0(3) 2_666 . ?
C1 Mo1 C2 88.96(18) 2_666 . ?
C1 Mo1 C2 91.04(18) . . ?
C1 Mo1 C2 91.04(18) 2_666 2_666 ?
C1 Mo1 C2 88.96(18) . 2_666 ?
C2 Mo1 C2 180 . 2_666 ?
C1 Mo1 Ge1 85.27(12) 2_666 . ?
C1 Mo1 Ge1 94.73(12) . . ?
C2 Mo1 Ge1 88.14(13) . . ?
C2 Mo1 Ge1 91.86(13) 2_666 . ?
C1 Mo1 Ge1 94.73(12) 2_666 2_666 ?
C1 Mo1 Ge1 85.27(12) . 2_666 ?
C2 Mo1 Ge1 91.86(13) . 2_666 ?
C2 Mo1 Ge1 88.14(13) 2_666 2_666 ?
Ge1 Mo1 Ge1 180 . 2_666 ?
N1 Ge1 N2 66.47(15) . . ?
N1 Ge1 C14 100.89(17) . . ?
N2 Ge1 C14 101.79(17) . . ?
N1 Ge1 Mo1 133.06(11) . . ?
N2 Ge1 Mo1 128.14(11) . . ?
C14 Ge1 Mo1 115.26(13) . . ?
C3 N1 C8 133.3(4) . . ?
C3 N1 Ge1 93.6(3) . . ?
C8 N1 Ge1 130.1(3) . . ?
C3 N2 C11 132.1(4) . . ?
C3 N2 Ge1 93.4(3) . . ?
C11 N2 Ge1 134.5(3) . . ?
C25 O4 C22 106.7(6) . . ?

