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

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1937808'
loop_
_audit_author_name
_audit_author_address
'Javier A. Cabeza'
;University of Oviedo
Spain
;
_audit_update_record             
;
2019-07-02 deposited with the CCDC.	2019-07-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H42 Ge N2 P2'
_chemical_formula_sum            'C25 H42 Ge N2 P2'
_chemical_formula_weight         505.13

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   11.4095(6)
_cell_length_b                   17.4206(7)
_cell_length_c                   14.3260(6)
_cell_angle_alpha                90
_cell_angle_beta                 112.581(6)
_cell_angle_gamma                90
_cell_volume                     2629.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5045
_cell_measurement_theta_min      4.1800
_cell_measurement_theta_max      69.2670

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_F_000             1072
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    2.825
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.67028
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14749
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         4.196
_diffrn_reflns_theta_max         69.581
_diffrn_reflns_theta_full        67.680
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4880
_reflns_number_gt                3594
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_cell_refinement       
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction        
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_structure_solution    'SIR-97 (Giacovazzo, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    
'MERCURY (Cambridge Crystallographic Data Centre: Cambridge, UK, 2019)'

_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)+(0.0467P)²+0.8339P] 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         4880
_refine_ls_number_parameters     281
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0437
_refine_ls_wR_factor_ref         0.1290
_refine_ls_wR_factor_gt          0.1163
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_restrained_S_all      1.139
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7413(5) -0.1604(3) 0.6659(3) 0.0515(11) Uani 1 1 d . . . . .
H1A H 0.6972 -0.1713 0.7112 0.077 Uiso 1 1 calc R U . . .
H1B H 0.8253 -0.1845 0.6926 0.077 Uiso 1 1 calc R U . . .
H1C H 0.6919 -0.1810 0.5986 0.077 Uiso 1 1 calc R U . . .
C2 C 0.6267(4) -0.0349(3) 0.6262(3) 0.0445(10) Uani 1 1 d . . . . .
H2A H 0.5702 -0.0557 0.5608 0.067 Uiso 1 1 calc R U . . .
H2B H 0.6367 0.0205 0.6199 0.067 Uiso 1 1 calc R U . . .
H2C H 0.5901 -0.0445 0.6768 0.067 Uiso 1 1 calc R U . . .
C3 C 0.7560(4) -0.0738(2) 0.6589(3) 0.0362(9) Uani 1 1 d . . . . .
H3 H 0.7879 -0.0648 0.6039 0.043 Uiso 1 1 calc R U . . .
C4 C 1.1253(4) 0.0098(3) 0.8537(4) 0.0551(12) Uani 1 1 d . . . . .
H4A H 1.1273 -0.0032 0.9209 0.083 Uiso 1 1 calc R U . . .
H4B H 1.0988 0.0633 0.8381 0.083 Uiso 1 1 calc R U . . .
H4C H 1.2102 0.0029 0.8529 0.083 Uiso 1 1 calc R U . . .
C5 C 1.0795(5) -0.1252(3) 0.7920(4) 0.0577(12) Uani 1 1 d . . . . .
H5A H 1.1633 -0.1280 0.7881 0.087 Uiso 1 1 calc R U . . .
H5B H 1.0199 -0.1580 0.7398 0.087 Uiso 1 1 calc R U . . .
H5C H 1.0858 -0.1426 0.8588 0.087 Uiso 1 1 calc R U . . .
C6 C 1.0322(4) -0.0423(2) 0.7755(3) 0.0400(9) Uani 1 1 d . . . . .
H6 H 1.0296 -0.0259 0.7079 0.048 Uiso 1 1 calc R U . . .
C7 C 0.8615(4) -0.0830(2) 0.8824(3) 0.0380(9) Uani 1 1 d . . . . .
H7A H 0.8566 -0.1389 0.8690 0.046 Uiso 1 1 calc R U . . .
H7B H 0.9362 -0.0723 0.9451 0.046 Uiso 1 1 calc R U . . .
C8 C 0.7420(4) -0.0544(2) 0.8910(3) 0.0381(9) Uani 1 1 d . . . . .
C9 C 0.6403(4) -0.0895(2) 0.9011(3) 0.0429(10) Uani 1 1 d . . . . .
H9 H 0.6329 -0.1424 0.9140 0.052 Uiso 1 1 calc R U . . .
C10 C 0.5478(4) -0.0317(2) 0.8889(3) 0.0421(10) Uani 1 1 d . . . . .
H10 H 0.4668 -0.0389 0.8920 0.050 Uiso 1 1 calc R U . . .
C11 C 0.5963(4) 0.0363(2) 0.8718(3) 0.0361(9) Uani 1 1 d . . . . .
C12 C 0.5420(4) 0.1158(2) 0.8452(3) 0.0375(9) Uani 1 1 d . . . . .
C13 C 0.4011(4) 0.1157(3) 0.8265(3) 0.0467(10) Uani 1 1 d . . . . .
H13A H 0.3562 0.0798 0.7717 0.070 Uiso 1 1 calc R U . . .
H13B H 0.3664 0.1674 0.8076 0.070 Uiso 1 1 calc R U . . .
H13C H 0.3901 0.0997 0.8882 0.070 Uiso 1 1 calc R U . . .
C14 C 0.6101(4) 0.1710(3) 0.9336(3) 0.0479(11) Uani 1 1 d . . . . .
H14A H 0.5962 0.1540 0.9938 0.072 Uiso 1 1 calc R U . . .
H14B H 0.5761 0.2229 0.9154 0.072 Uiso 1 1 calc R U . . .
H14C H 0.7013 0.1711 0.9480 0.072 Uiso 1 1 calc R U . . .
C15 C 0.5607(4) 0.1434(2) 0.7510(3) 0.0359(8) Uani 1 1 d . . . . .
C16 C 0.4778(4) 0.1789(2) 0.6653(3) 0.0403(9) Uani 1 1 d . . . . .
H16 H 0.3895 0.1864 0.6478 0.048 Uiso 1 1 calc R U . . .
C17 C 0.5490(4) 0.2024(2) 0.6078(3) 0.0405(9) Uani 1 1 d . . . . .
H17 H 0.5165 0.2282 0.5446 0.049 Uiso 1 1 calc R U . . .
C18 C 0.6723(4) 0.1813(2) 0.6595(3) 0.0355(8) Uani 1 1 d . . . . .
C19 C 0.7873(4) 0.1979(2) 0.6367(3) 0.0418(10) Uani 1 1 d . . . . .
H19A H 0.8575 0.2124 0.7006 0.050 Uiso 1 1 calc R U . . .
H19B H 0.7689 0.2429 0.5911 0.050 Uiso 1 1 calc R U . . .
C20 C 0.7083(4) 0.1141(3) 0.4529(3) 0.0448(10) Uani 1 1 d . . . . .
H20 H 0.6305 0.1100 0.4688 0.054 Uiso 1 1 calc R U . . .
C21 C 0.7101(5) 0.0405(3) 0.3950(3) 0.0566(12) Uani 1 1 d . . . . .
H21A H 0.6313 0.0368 0.3348 0.085 Uiso 1 1 calc R U . . .
H21B H 0.7175 -0.0040 0.4386 0.085 Uiso 1 1 calc R U . . .
H21C H 0.7827 0.0418 0.3744 0.085 Uiso 1 1 calc R U . . .
C22 C 0.6864(5) 0.1845(3) 0.3845(4) 0.0641(14) Uani 1 1 d . . . . .
H22A H 0.7568 0.1897 0.3618 0.096 Uiso 1 1 calc R U . . .
H22B H 0.6817 0.2305 0.4223 0.096 Uiso 1 1 calc R U . . .
H22C H 0.6066 0.1784 0.3257 0.096 Uiso 1 1 calc R U . . .
C23 C 0.9716(4) 0.1695(2) 0.5531(3) 0.0418(9) Uani 1 1 d . . . . .
H23 H 0.9347 0.2164 0.5122 0.050 Uiso 1 1 calc R U . . .
C24 C 1.0266(5) 0.1192(3) 0.4943(4) 0.0642(15) Uani 1 1 d . . . . .
H24A H 1.0981 0.1456 0.4866 0.096 Uiso 1 1 calc R U . . .
H24B H 0.9612 0.1085 0.4274 0.096 Uiso 1 1 calc R U . . .
H24C H 1.0560 0.0708 0.5307 0.096 Uiso 1 1 calc R U . . .
C25 C 1.0755(5) 0.1940(4) 0.6514(4) 0.0717(16) Uani 1 1 d . . . . .
H25A H 1.1086 0.1488 0.6943 0.108 Uiso 1 1 calc R U . . .
H25B H 1.0409 0.2304 0.6864 0.108 Uiso 1 1 calc R U . . .
H25C H 1.1442 0.2185 0.6373 0.108 Uiso 1 1 calc R U . . .
Ge1 Ge 0.82933(4) 0.09483(3) 0.84660(3) 0.03599(15) Uani 1 1 d . . . . .
P1 P 0.87136(9) -0.02888(6) 0.77435(7) 0.0332(2) Uani 1 1 d . . . . .
P2 P 0.84322(10) 0.11823(6) 0.57776(7) 0.0356(2) Uani 1 1 d . . . . .
N1 N 0.7163(3) 0.02281(18) 0.8750(2) 0.0356(7) Uani 1 1 d . . . . .
N2 N 0.6809(3) 0.14331(18) 0.7471(2) 0.0358(7) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C3 1.525(6) . ?
C2 C3 1.524(6) . ?
C3 P1 1.846(4) . ?
C4 C6 1.515(6) . ?
C5 C6 1.528(6) . ?
C6 P1 1.843(4) . ?
C7 C8 1.500(5) . ?
C7 P1 1.852(4) . ?
C8 C9 1.368(6) . ?
C8 N1 1.377(5) . ?
C9 C10 1.420(6) . ?
C10 C11 1.369(6) . ?
C11 N1 1.373(5) . ?
C11 C12 1.506(6) . ?
C12 C15 1.522(5) . ?
C12 C13 1.525(6) . ?
C12 C14 1.541(6) . ?
C15 C16 1.376(6) . ?
C15 N2 1.395(5) . ?
C16 C17 1.421(6) . ?
C17 C18 1.364(6) . ?
C18 N2 1.389(5) . ?
C18 C19 1.497(5) . ?
C19 P2 1.860(4) . ?
C20 C22 1.528(6) . ?
C20 C21 1.531(6) . ?
C20 P2 1.861(4) . ?
C23 C24 1.509(6) . ?
C23 C25 1.513(6) . ?
C23 P2 1.861(4) . ?
Ge1 N2 1.939(3) . ?
Ge1 N1 1.950(3) . ?
Ge1 P1 2.5154(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C3 C1 110.0(3) . . ?
C2 C3 P1 111.1(3) . . ?
C1 C3 P1 114.8(3) . . ?
C4 C6 C5 110.2(4) . . ?
C4 C6 P1 110.1(3) . . ?
C5 C6 P1 114.4(3) . . ?
C8 C7 P1 104.4(3) . . ?
C9 C8 N1 108.6(3) . . ?
C9 C8 C7 134.1(4) . . ?
N1 C8 C7 116.8(3) . . ?
C8 C9 C10 106.9(4) . . ?
C11 C10 C9 107.7(4) . . ?
C10 C11 N1 108.2(3) . . ?
C10 C11 C12 133.3(4) . . ?
N1 C11 C12 118.3(3) . . ?
C11 C12 C15 109.3(3) . . ?
C11 C12 C13 110.3(3) . . ?
C15 C12 C13 110.0(3) . . ?
C11 C12 C14 109.7(3) . . ?
C15 C12 C14 109.5(3) . . ?
C13 C12 C14 108.1(3) . . ?
C16 C15 N2 108.3(3) . . ?
C16 C15 C12 130.6(4) . . ?
N2 C15 C12 120.7(3) . . ?
C15 C16 C17 107.3(4) . . ?
C18 C17 C16 107.9(3) . . ?
C17 C18 N2 108.6(3) . . ?
C17 C18 C19 129.6(4) . . ?
N2 C18 C19 121.6(4) . . ?
C18 C19 P2 115.9(3) . . ?
C22 C20 C21 111.0(4) . . ?
C22 C20 P2 117.1(3) . . ?
C21 C20 P2 112.0(3) . . ?
C24 C23 C25 109.8(4) . . ?
C24 C23 P2 110.7(3) . . ?
C25 C23 P2 110.5(3) . . ?
N2 Ge1 N1 88.45(13) . . ?
N2 Ge1 P1 108.73(9) . . ?
N1 Ge1 P1 77.31(9) . . ?
C6 P1 C3 108.61(18) . . ?
C6 P1 C7 107.93(18) . . ?
C3 P1 C7 106.34(18) . . ?
C6 P1 Ge1 116.83(14) . . ?
C3 P1 Ge1 123.30(13) . . ?
C7 P1 Ge1 90.55(13) . . ?
C19 P2 C20 99.46(19) . . ?
C19 P2 C23 99.21(18) . . ?
C20 P2 C23 104.88(19) . . ?
C11 N1 C8 108.6(3) . . ?
C11 N1 Ge1 127.9(3) . . ?
C8 N1 Ge1 123.2(3) . . ?
C18 N2 C15 107.9(3) . . ?
C18 N2 Ge1 127.7(3) . . ?
C15 N2 Ge1 124.4(2) . . ?

_refine_diff_density_max         0.403
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.069

_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 1937809'
loop_
_audit_author_name
_audit_author_address
'Javier A. Cabeza'
;University of Oviedo
Spain
;
_audit_update_record             
;
2019-07-02 deposited with the CCDC.	2019-07-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C43 H57 Cl Cu Ge N2 P3'
_chemical_formula_sum            'C43 H57 Cl Cu Ge N2 P3'
_chemical_formula_weight         866.39

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'
Cu Cu -1.9646 0.5888 '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'

_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                   15.9072(2)
_cell_length_b                   13.5272(2)
_cell_length_c                   19.6745(2)
_cell_angle_alpha                90
_cell_angle_beta                 92.3280(10)
_cell_angle_gamma                90
_cell_volume                     4230.06(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    12693
_cell_measurement_theta_min      4.2740
_cell_measurement_theta_max      69.2430

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_F_000             1808
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    3.384
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.76219
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19099
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.780
_diffrn_reflns_theta_max         69.553
_diffrn_reflns_theta_full        67.680
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             7803
_reflns_number_gt                6919
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_cell_refinement       
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction        
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_structure_solution    'SIR-97 (Giacovazzo, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    
'MERCURY (Cambridge Crystallographic Data Centre: Cambridge, UK, 2019)'
_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)+(0.0353P)²+1.1100P] 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         7803
_refine_ls_number_parameters     462
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0281
_refine_ls_wR_factor_ref         0.0721
_refine_ls_wR_factor_gt          0.0689
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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
C1 C 0.45837(13) 0.59807(16) 0.68440(11) 0.0309(5) Uani 1 1 d . . . . .
H1A H 0.4296 0.5642 0.6461 0.046 Uiso 1 1 calc R U . . .
H1B H 0.4334 0.6636 0.6902 0.046 Uiso 1 1 calc R U . . .
H1C H 0.5182 0.6052 0.6754 0.046 Uiso 1 1 calc R U . . .
C2 C 0.49331(13) 0.58871(19) 0.81020(12) 0.0375(5) Uani 1 1 d . . . . .
H2A H 0.4867 0.5490 0.8513 0.056 Uiso 1 1 calc R U . . .
H2B H 0.5533 0.5958 0.8017 0.056 Uiso 1 1 calc R U . . .
H2C H 0.4685 0.6542 0.8165 0.056 Uiso 1 1 calc R U . . .
C3 C 0.44884(12) 0.53732(16) 0.74948(10) 0.0262(4) Uani 1 1 d . . . . .
H3 H 0.4804 0.4744 0.7425 0.031 Uiso 1 1 calc R U . . .
C4 C 0.34990(17) 0.4545(2) 0.90638(11) 0.0436(6) Uani 1 1 d . . . . .
H4A H 0.3067 0.5053 0.9117 0.065 Uiso 1 1 calc R U . . .
H4B H 0.3421 0.4016 0.9396 0.065 Uiso 1 1 calc R U . . .
H4C H 0.4058 0.4840 0.9140 0.065 Uiso 1 1 calc R U . . .
C5 C 0.40847(15) 0.33202(18) 0.82358(12) 0.0398(5) Uani 1 1 d . . . . .
H5A H 0.4018 0.3063 0.7771 0.060 Uiso 1 1 calc R U . . .
H5B H 0.4648 0.3605 0.8305 0.060 Uiso 1 1 calc R U . . .
H5C H 0.4012 0.2781 0.8561 0.060 Uiso 1 1 calc R U . . .
C6 C 0.34221(13) 0.41188(16) 0.83449(10) 0.0286(4) Uani 1 1 d . . . . .
H6 H 0.2870 0.3765 0.8320 0.034 Uiso 1 1 calc R U . . .
C7 C 0.28589(12) 0.61351(15) 0.79465(10) 0.0242(4) Uani 1 1 d . . . . .
H7A H 0.2250 0.6004 0.7981 0.029 Uiso 1 1 calc R U . . .
H7B H 0.3094 0.6279 0.8410 0.029 Uiso 1 1 calc R U . . .
C8 C 0.29723(12) 0.70273(15) 0.75054(10) 0.0243(4) Uani 1 1 d . . . . .
C9 C 0.33998(13) 0.78770(16) 0.76663(11) 0.0300(4) Uani 1 1 d . . . . .
H9 H 0.3624 0.8060 0.8103 0.036 Uiso 1 1 calc R U . . .
C10 C 0.34470(14) 0.84360(16) 0.70586(12) 0.0333(5) Uani 1 1 d . . . . .
H10 H 0.3710 0.9062 0.7016 0.040 Uiso 1 1 calc R U . . .
C11 C 0.30460(12) 0.79131(15) 0.65434(11) 0.0281(4) Uani 1 1 d . . . . .
C12 C 0.29527(13) 0.81498(16) 0.57866(12) 0.0326(5) Uani 1 1 d . . . . .
C13 C 0.21132(16) 0.86939(19) 0.56270(15) 0.0468(6) Uani 1 1 d . . . . .
H13A H 0.2087 0.9290 0.5909 0.070 Uiso 1 1 calc R U . . .
H13B H 0.2078 0.8880 0.5145 0.070 Uiso 1 1 calc R U . . .
H13C H 0.1642 0.8257 0.5726 0.070 Uiso 1 1 calc R U . . .
C14 C 0.36764(17) 0.88439(19) 0.56066(14) 0.0460(6) Uani 1 1 d . . . . .
H14A H 0.3654 0.9445 0.5883 0.069 Uiso 1 1 calc R U . . .
H14B H 0.4216 0.8509 0.5698 0.069 Uiso 1 1 calc R U . . .
H14C H 0.3621 0.9020 0.5124 0.069 Uiso 1 1 calc R U . . .
C15 C 0.30001(12) 0.72254(16) 0.53526(10) 0.0274(4) Uani 1 1 d . . . . .
C16 C 0.33946(13) 0.70735(18) 0.47524(11) 0.0349(5) Uani 1 1 d . . . . .
H16 H 0.3721 0.7545 0.4521 0.042 Uiso 1 1 calc R U . . .
C17 C 0.32283(13) 0.60923(18) 0.45422(11) 0.0324(5) Uani 1 1 d . . . . .
H17 H 0.3422 0.5786 0.4143 0.039 Uiso 1 1 calc R U . . .
C18 C 0.27388(11) 0.56612(16) 0.50145(9) 0.0241(4) Uani 1 1 d . . . . .
C19 C 0.23991(12) 0.46342(16) 0.50354(9) 0.0263(4) Uani 1 1 d . . . . .
H19A H 0.2477 0.4320 0.4588 0.032 Uiso 1 1 calc R U . . .
H19B H 0.1787 0.4671 0.5103 0.032 Uiso 1 1 calc R U . . .
C20 C 0.40168(12) 0.39835(16) 0.55443(10) 0.0275(4) Uani 1 1 d . . . . .
H20 H 0.4119 0.4713 0.5559 0.033 Uiso 1 1 calc R U . . .
C21 C 0.42878(15) 0.3650(2) 0.48429(11) 0.0407(6) Uani 1 1 d . . . . .
H21A H 0.3910 0.3938 0.4491 0.061 Uiso 1 1 calc R U . . .
H21B H 0.4865 0.3871 0.4775 0.061 Uiso 1 1 calc R U . . .
H21C H 0.4262 0.2927 0.4814 0.061 Uiso 1 1 calc R U . . .
C22 C 0.45928(14) 0.3548(2) 0.61112(11) 0.0379(5) Uani 1 1 d . . . . .
H22A H 0.4406 0.3773 0.6554 0.057 Uiso 1 1 calc R U . . .
H22B H 0.4569 0.2825 0.6091 0.057 Uiso 1 1 calc R U . . .
H22C H 0.5172 0.3768 0.6051 0.057 Uiso 1 1 calc R U . . .
C23 C 0.26203(17) 0.25775(18) 0.53547(12) 0.0413(6) Uani 1 1 d . . . . .
H23 H 0.2789 0.2573 0.4871 0.050 Uiso 1 1 calc R U . . .
C24 C 0.1682(2) 0.2393(3) 0.53500(19) 0.0728(10) Uani 1 1 d . . . . .
H24A H 0.1558 0.1740 0.5154 0.109 Uiso 1 1 calc R U . . .
H24B H 0.1390 0.2902 0.5076 0.109 Uiso 1 1 calc R U . . .
H24C H 0.1490 0.2416 0.5817 0.109 Uiso 1 1 calc R U . . .
C25 C 0.3105(3) 0.1750(2) 0.57214(15) 0.0653(9) Uani 1 1 d . . . . .
H25A H 0.3040 0.1811 0.6213 0.098 Uiso 1 1 calc R U . . .
H25B H 0.3702 0.1797 0.5622 0.098 Uiso 1 1 calc R U . . .
H25C H 0.2884 0.1109 0.5565 0.098 Uiso 1 1 calc R U . . .
C26 C 0.03648(12) 0.36235(15) 0.68234(11) 0.0263(4) Uani 1 1 d . . . . .
C27 C 0.03374(14) 0.38451(18) 0.61405(11) 0.0366(5) Uani 1 1 d . . . . .
H27 H 0.0825 0.4099 0.5938 0.044 Uiso 1 1 calc R U . . .
C28 C -0.03959(17) 0.3702(2) 0.57437(14) 0.0496(7) Uani 1 1 d . . . . .
H28 H -0.0405 0.3853 0.5272 0.060 Uiso 1 1 calc R U . . .
C29 C -0.11049(16) 0.33440(19) 0.60304(17) 0.0528(7) Uani 1 1 d . . . . .
H29 H -0.1597 0.3217 0.5755 0.063 Uiso 1 1 calc R U . . .
C30 C -0.10997(14) 0.31697(19) 0.67208(17) 0.0498(7) Uani 1 1 d . . . . .
H30 H -0.1599 0.2951 0.6923 0.060 Uiso 1 1 calc R U . . .
C31 C -0.03723(13) 0.33100(17) 0.71230(13) 0.0385(5) Uani 1 1 d . . . . .
H31 H -0.0375 0.3194 0.7599 0.046 Uiso 1 1 calc R U . . .
C32 C 0.16012(12) 0.25117(15) 0.76487(10) 0.0236(4) Uani 1 1 d . . . . .
C33 C 0.23418(14) 0.20765(17) 0.74654(12) 0.0365(5) Uani 1 1 d . . . . .
H33 H 0.2714 0.2435 0.7191 0.044 Uiso 1 1 calc R U . . .
C34 C 0.25556(17) 0.1125(2) 0.76728(15) 0.0504(7) Uani 1 1 d . . . . .
H34 H 0.3068 0.0837 0.7538 0.060 Uiso 1 1 calc R U . . .
C35 C 0.20265(15) 0.05990(18) 0.80725(13) 0.0402(5) Uani 1 1 d . . . . .
H35 H 0.2167 -0.0055 0.8211 0.048 Uiso 1 1 calc R U . . .
C36 C 0.12914(14) 0.10262(18) 0.82714(13) 0.0410(6) Uani 1 1 d . . . . .
H36 H 0.0926 0.0667 0.8551 0.049 Uiso 1 1 calc R U . . .
C37 C 0.10803(13) 0.19742(18) 0.80669(13) 0.0383(5) Uani 1 1 d . . . . .
H37 H 0.0574 0.2264 0.8213 0.046 Uiso 1 1 calc R U . . .
C38 C 0.10000(12) 0.44490(15) 0.80479(10) 0.0253(4) Uani 1 1 d . . . . .
C39 C 0.05075(15) 0.52815(17) 0.79148(11) 0.0351(5) Uani 1 1 d . . . . .
H39 H 0.0369 0.5460 0.7457 0.042 Uiso 1 1 calc R U . . .
C40 C 0.02150(18) 0.58538(18) 0.84390(13) 0.0454(6) Uani 1 1 d . . . . .
H40 H -0.0132 0.6410 0.8338 0.054 Uiso 1 1 calc R U . . .
C41 C 0.04239(19) 0.5621(2) 0.91020(13) 0.0480(6) Uani 1 1 d . . . . .
H41 H 0.0220 0.6012 0.9461 0.058 Uiso 1 1 calc R U . . .
C42 C 0.09305(17) 0.4820(2) 0.92423(12) 0.0455(6) Uani 1 1 d . . . . .
H42 H 0.1091 0.4670 0.9701 0.055 Uiso 1 1 calc R U . . .
C43 C 0.12131(14) 0.42239(18) 0.87217(11) 0.0349(5) Uani 1 1 d . . . . .
H43 H 0.1552 0.3662 0.8828 0.042 Uiso 1 1 calc R U . . .
Cl1 Cl 0.08348(3) 0.66894(4) 0.62013(3) 0.03445(12) Uani 1 1 d . . . . .
Cu1 Cu 0.24773(2) 0.44137(2) 0.67486(2) 0.01931(7) Uani 1 1 d . . . . .
Ge1 Ge 0.21308(2) 0.60175(2) 0.63603(2) 0.01938(7) Uani 1 1 d . . . . .
N1 N 0.27309(10) 0.70536(12) 0.68192(8) 0.0242(3) Uani 1 1 d . . . . .
N2 N 0.25913(10) 0.63582(13) 0.55138(8) 0.0235(3) Uani 1 1 d . . . . .
P1 P 0.33759(3) 0.50058(4) 0.76182(2) 0.01972(10) Uani 1 1 d . . . . .
P2 P 0.28866(3) 0.38246(4) 0.57091(2) 0.02276(11) Uani 1 1 d . . . . .
P3 P 0.13655(3) 0.37525(4) 0.73152(2) 0.02029(10) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C3 1.534(3) . ?
C2 C3 1.530(3) . ?
C3 P1 1.8633(19) . ?
C4 C6 1.528(3) . ?
C5 C6 1.530(3) . ?
C6 P1 1.866(2) . ?
C7 C8 1.502(3) . ?
C7 P1 1.863(2) . ?
C8 C9 1.366(3) . ?
C8 N1 1.389(3) . ?
C9 C10 1.419(3) . ?
C10 C11 1.372(3) . ?
C11 N1 1.386(3) . ?
C11 C12 1.524(3) . ?
C12 C15 1.518(3) . ?
C12 C14 1.538(3) . ?
C12 C13 1.546(3) . ?
C15 C16 1.375(3) . ?
C15 N2 1.384(3) . ?
C16 C17 1.412(4) . ?
C17 C18 1.367(3) . ?
C18 N2 1.388(3) . ?
C18 C19 1.492(3) . ?
C19 P2 1.864(2) . ?
C20 C21 1.530(3) . ?
C20 C22 1.532(3) . ?
C20 P2 1.852(2) . ?
C23 C24 1.513(4) . ?
C23 C25 1.524(4) . ?
C23 P2 1.867(2) . ?
C26 C27 1.376(3) . ?
C26 C31 1.400(3) . ?
C26 P3 1.837(2) . ?
C27 C28 1.390(3) . ?
C28 C29 1.370(4) . ?
C29 C30 1.378(4) . ?
C30 C31 1.388(3) . ?
C32 C33 1.378(3) . ?
C32 C37 1.396(3) . ?
C32 P3 1.835(2) . ?
C33 C34 1.389(3) . ?
C34 C35 1.373(4) . ?
C35 C36 1.375(4) . ?
C36 C37 1.381(3) . ?
C38 C43 1.389(3) . ?
C38 C39 1.391(3) . ?
C38 P3 1.836(2) . ?
C39 C40 1.385(3) . ?
C40 C41 1.370(4) . ?
C41 C42 1.372(4) . ?
C42 C43 1.393(3) . ?
Cl1 Ge1 2.2631(5) . ?
Cu1 P3 2.3089(5) . ?
Cu1 P2 2.3128(5) . ?
Cu1 P1 2.3267(5) . ?
Cu1 Ge1 2.3580(3) . ?
Ge1 N1 1.9028(17) . ?
Ge1 N2 1.9032(16) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C3 C1 110.48(18) . . ?
C2 C3 P1 115.52(14) . . ?
C1 C3 P1 112.22(13) . . ?
C4 C6 C5 111.51(19) . . ?
C4 C6 P1 117.76(16) . . ?
C5 C6 P1 110.64(14) . . ?
C8 C7 P1 113.18(13) . . ?
C9 C8 N1 108.61(18) . . ?
C9 C8 C7 127.79(18) . . ?
N1 C8 C7 123.18(17) . . ?
C8 C9 C10 107.22(18) . . ?
C11 C10 C9 107.99(19) . . ?
C10 C11 N1 107.94(18) . . ?
C10 C11 C12 129.59(19) . . ?
N1 C11 C12 122.44(18) . . ?
C15 C12 C11 111.80(17) . . ?
C15 C12 C14 108.58(19) . . ?
C11 C12 C14 108.00(18) . . ?
C15 C12 C13 109.89(19) . . ?
C11 C12 C13 110.33(19) . . ?
C14 C12 C13 108.13(19) . . ?
C16 C15 N2 107.8(2) . . ?
C16 C15 C12 129.9(2) . . ?
N2 C15 C12 122.33(18) . . ?
C15 C16 C17 107.79(19) . . ?
C18 C17 C16 107.87(19) . . ?
C17 C18 N2 107.98(19) . . ?
C17 C18 C19 129.27(19) . . ?
N2 C18 C19 122.75(16) . . ?
C18 C19 P2 115.22(13) . . ?
C21 C20 C22 111.17(17) . . ?
C21 C20 P2 115.76(16) . . ?
C22 C20 P2 112.57(14) . . ?
C24 C23 C25 111.2(3) . . ?
C24 C23 P2 111.11(18) . . ?
C25 C23 P2 112.60(19) . . ?
C27 C26 C31 118.9(2) . . ?
C27 C26 P3 119.09(16) . . ?
C31 C26 P3 121.99(17) . . ?
C26 C27 C28 120.7(2) . . ?
C29 C28 C27 120.3(3) . . ?
C28 C29 C30 119.6(2) . . ?
C29 C30 C31 120.7(2) . . ?
C30 C31 C26 119.6(2) . . ?
C33 C32 C37 117.8(2) . . ?
C33 C32 P3 117.49(15) . . ?
C37 C32 P3 124.72(16) . . ?
C32 C33 C34 121.4(2) . . ?
C35 C34 C33 120.0(2) . . ?
C34 C35 C36 119.6(2) . . ?
C35 C36 C37 120.4(2) . . ?
C36 C37 C32 120.8(2) . . ?
C43 C38 C39 118.1(2) . . ?
C43 C38 P3 124.34(16) . . ?
C39 C38 P3 117.49(16) . . ?
C40 C39 C38 121.1(2) . . ?
C41 C40 C39 120.3(2) . . ?
C40 C41 C42 119.4(2) . . ?
C41 C42 C43 120.9(2) . . ?
C38 C43 C42 120.1(2) . . ?
P3 Cu1 P2 122.83(2) . . ?
P3 Cu1 P1 103.777(19) . . ?
P2 Cu1 P1 125.60(2) . . ?
P3 Cu1 Ge1 109.832(17) . . ?
P2 Cu1 Ge1 95.799(16) . . ?
P1 Cu1 Ge1 92.867(16) . . ?
N1 Ge1 N2 91.92(7) . . ?
N1 Ge1 Cl1 101.91(5) . . ?
N2 Ge1 Cl1 99.36(5) . . ?
N1 Ge1 Cu1 114.70(5) . . ?
N2 Ge1 Cu1 114.40(5) . . ?
Cl1 Ge1 Cu1 127.872(18) . . ?
C11 N1 C8 108.18(17) . . ?
C11 N1 Ge1 127.93(14) . . ?
C8 N1 Ge1 123.78(14) . . ?
C15 N2 C18 108.60(16) . . ?
C15 N2 Ge1 127.35(14) . . ?
C18 N2 Ge1 122.47(13) . . ?
C7 P1 C3 105.16(9) . . ?
C7 P1 C6 105.42(9) . . ?
C3 P1 C6 105.26(9) . . ?
C7 P1 Cu1 105.69(6) . . ?
C3 P1 Cu1 123.67(6) . . ?
C6 P1 Cu1 110.24(7) . . ?
C20 P2 C19 100.72(9) . . ?
C20 P2 C23 104.27(11) . . ?
C19 P2 C23 100.59(10) . . ?
C20 P2 Cu1 115.15(7) . . ?
C19 P2 Cu1 107.60(7) . . ?
C23 P2 Cu1 125.01(8) . . ?
C32 P3 C38 104.79(9) . . ?
C32 P3 C26 105.16(9) . . ?
C38 P3 C26 99.62(9) . . ?
C32 P3 Cu1 112.18(6) . . ?
C38 P3 Cu1 116.96(7) . . ?
C26 P3 Cu1 116.54(7) . . ?

_refine_diff_density_max         0.386
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.052

_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 1937810'
loop_
_audit_author_name
_audit_author_address
'Javier A. Cabeza'
;University of Oviedo
Spain
;
_audit_update_record             
;
2019-07-02 deposited with the CCDC.	2019-07-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H42 Ag Cl Ge N2 P2, C D2 Cl2'
_chemical_formula_sum            'C26 H42 Ag Cl3 D2 Ge N2 P2'
_chemical_formula_weight         735.39

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'
D D 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 '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'

_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                   11.156(5)
_cell_length_b                   11.334(5)
_cell_length_c                   13.448(5)
_cell_angle_alpha                91.841(5)
_cell_angle_beta                 109.257(5)
_cell_angle_gamma                92.640(5)
_cell_volume                     1601.5(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    152(2)
_cell_measurement_reflns_used    11248
_cell_measurement_theta_min      3.4680
_cell_measurement_theta_max      69.4510

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_F_000             748
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    9.439
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.34447
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      152(2)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15491
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.486
_diffrn_reflns_theta_max         69.494
_diffrn_reflns_theta_full        67.680
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5943
_reflns_number_gt                5570
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_cell_refinement       
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction        
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_structure_solution    'SIR-97 (Giacovazzo, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    
'MERCURY (Cambridge Crystallographic Data Centre: Cambridge, UK, 2019)'
_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)+(0.0502P)²+1.6273P] 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         5943
_refine_ls_number_parameters     326
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0353
_refine_ls_wR_factor_ref         0.0928
_refine_ls_wR_factor_gt          0.0905
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.0451(3) 0.1704(4) 0.7236(3) 0.0456(9) Uani 1 1 d . . . . .
H1A H 1.1151 0.1256 0.7164 0.068 Uiso 1 1 calc R U . . .
H1B H 1.0316 0.1527 0.7901 0.068 Uiso 1 1 calc R U . . .
H1C H 1.0663 0.2552 0.7233 0.068 Uiso 1 1 calc R U . . .
C2 C 0.9362(4) 0.1632(4) 0.5254(3) 0.0438(9) Uani 1 1 d . . . . .
H2A H 0.9512 0.2487 0.5229 0.066 Uiso 1 1 calc R U . . .
H2B H 0.8578 0.1362 0.4688 0.066 Uiso 1 1 calc R U . . .
H2C H 1.0079 0.1227 0.5163 0.066 Uiso 1 1 calc R U . . .
C3 C 0.9235(3) 0.1352(3) 0.6312(3) 0.0324(7) Uani 1 1 d . . . . .
H3 H 0.9123 0.0471 0.6305 0.039 Uiso 1 1 calc R U . . .
C4 C 0.8580(4) 0.4305(3) 0.6692(4) 0.0466(9) Uani 1 1 d . . . . .
H4A H 0.8444 0.5085 0.6395 0.070 Uiso 1 1 calc R U . . .
H4B H 0.9431 0.4071 0.6738 0.070 Uiso 1 1 calc R U . . .
H4C H 0.8506 0.4338 0.7399 0.070 Uiso 1 1 calc R U . . .
C5 C 0.6243(3) 0.3763(3) 0.5862(3) 0.0400(8) Uani 1 1 d . . . . .
H5A H 0.6105 0.3731 0.6544 0.060 Uiso 1 1 calc R U . . .
H5B H 0.5618 0.3222 0.5345 0.060 Uiso 1 1 calc R U . . .
H5C H 0.6148 0.4571 0.5621 0.060 Uiso 1 1 calc R U . . .
C6 C 0.7581(3) 0.3399(3) 0.5983(3) 0.0304(7) Uani 1 1 d . . . . .
H6 H 0.7681 0.3359 0.5270 0.036 Uiso 1 1 calc R U . . .
C7 C 0.6496(3) 0.0955(3) 0.5644(2) 0.0241(6) Uani 1 1 d . . . . .
H7A H 0.5677 0.1280 0.5616 0.029 Uiso 1 1 calc R U . . .
H7B H 0.6550 0.0952 0.4924 0.029 Uiso 1 1 calc R U . . .
C8 C 0.6516(3) -0.0293(3) 0.5990(2) 0.0235(6) Uani 1 1 d . . . . .
C9 C 0.7006(3) -0.1248(3) 0.5642(3) 0.0284(6) Uani 1 1 d . . . . .
H9 H 0.7405 -0.1255 0.5117 0.034 Uiso 1 1 calc R U . . .
C10 C 0.6801(3) -0.2226(3) 0.6215(3) 0.0304(7) Uani 1 1 d . . . . .
H10 H 0.7041 -0.3009 0.6143 0.036 Uiso 1 1 calc R U . . .
C11 C 0.6199(3) -0.1839(3) 0.6891(2) 0.0245(6) Uani 1 1 d . . . . .
C12 C 0.5749(3) -0.2508(3) 0.7676(3) 0.0280(6) Uani 1 1 d . . . . .
C13 C 0.4298(3) -0.2787(3) 0.7232(3) 0.0360(7) Uani 1 1 d . . . . .
H13A H 0.4025 -0.3225 0.7744 0.054 Uiso 1 1 calc R U . . .
H13B H 0.4084 -0.3266 0.6571 0.054 Uiso 1 1 calc R U . . .
H13C H 0.3864 -0.2047 0.7100 0.054 Uiso 1 1 calc R U . . .
C14 C 0.6370(4) -0.3699(3) 0.7839(3) 0.0393(8) Uani 1 1 d . . . . .
H14A H 0.7297 -0.3561 0.8120 0.059 Uiso 1 1 calc R U . . .
H14B H 0.6129 -0.4154 0.7163 0.059 Uiso 1 1 calc R U . . .
H14C H 0.6079 -0.4143 0.8339 0.059 Uiso 1 1 calc R U . . .
C15 C 0.6124(3) -0.1811(3) 0.8725(2) 0.0241(6) Uani 1 1 d . . . . .
C16 C 0.6629(3) -0.2196(3) 0.9722(3) 0.0286(6) Uani 1 1 d . . . . .
H16 H 0.6806 -0.2988 0.9904 0.034 Uiso 1 1 calc R U . . .
C17 C 0.6841(3) -0.1200(3) 1.0438(2) 0.0269(6) Uani 1 1 d . . . . .
H17 H 0.7191 -0.1201 1.1185 0.032 Uiso 1 1 calc R U . . .
C18 C 0.6447(3) -0.0237(3) 0.9852(2) 0.0231(6) Uani 1 1 d . . . . .
C19 C 0.6504(3) 0.1028(3) 1.0234(2) 0.0247(6) Uani 1 1 d . . . . .
H19A H 0.6544 0.1052 1.0981 0.030 Uiso 1 1 calc R U . . .
H19B H 0.5711 0.1388 0.9821 0.030 Uiso 1 1 calc R U . . .
C20 C 0.9255(3) 0.1281(3) 1.1088(3) 0.0366(8) Uani 1 1 d . . . . .
H20 H 0.9067 0.0405 1.1004 0.044 Uiso 1 1 calc R U . . .
C21 C 1.0485(4) 0.1505(5) 1.0832(4) 0.0563(11) Uani 1 1 d . . . . .
H21A H 1.0705 0.2357 1.0884 0.084 Uiso 1 1 calc R U . . .
H21B H 1.0360 0.1193 1.0115 0.084 Uiso 1 1 calc R U . . .
H21C H 1.1175 0.1107 1.1334 0.084 Uiso 1 1 calc R U . . .
C22 C 0.9425(4) 0.1615(4) 1.2233(3) 0.0468(9) Uani 1 1 d . . . . .
H22A H 1.0128 0.1196 1.2696 0.070 Uiso 1 1 calc R U . . .
H22B H 0.8640 0.1395 1.2377 0.070 Uiso 1 1 calc R U . . .
H22C H 0.9615 0.2470 1.2364 0.070 Uiso 1 1 calc R U . . .
C23 C 0.7714(3) 0.3410(3) 1.0642(3) 0.0348(7) Uani 1 1 d . . . . .
H23 H 0.7711 0.3350 1.1381 0.042 Uiso 1 1 calc R U . . .
C24 C 0.6449(4) 0.3879(3) 0.9975(4) 0.0491(10) Uani 1 1 d . . . . .
H24A H 0.6387 0.4688 1.0226 0.074 Uiso 1 1 calc R U . . .
H24B H 0.5744 0.3371 1.0036 0.074 Uiso 1 1 calc R U . . .
H24C H 0.6407 0.3878 0.9235 0.074 Uiso 1 1 calc R U . . .
C25 C 0.8825(4) 0.4259(4) 1.0657(4) 0.0552(11) Uani 1 1 d . . . . .
H25A H 0.8850 0.4317 0.9939 0.083 Uiso 1 1 calc R U . . .
H25B H 0.9623 0.3961 1.1109 0.083 Uiso 1 1 calc R U . . .
H25C H 0.8713 0.5042 1.0933 0.083 Uiso 1 1 calc R U . . .
C26 C 0.3039(6) 0.3449(7) 0.6530(6) 0.096(2) Uani 1 1 d . . . . .
D26A H 0.2686 0.2620 0.6392 0.116 Uiso 1 1 calc R U . . .
D26B H 0.3776 0.3517 0.6275 0.116 Uiso 1 1 calc R U . . .
Ag1 Ag 0.77184(2) 0.19020(2) 0.82974(2) 0.03005(9) Uani 1 1 d . . . . .
Cl1 Cl 0.33555(7) 0.01609(7) 0.70079(6) 0.03003(17) Uani 1 1 d . . . . .
Cl2 Cl 0.3544(2) 0.37706(18) 0.78394(14) 0.1237(8) Uani 1 1 d . . . . .
Cl3 Cl 0.1911(2) 0.4353(2) 0.58407(18) 0.1477(11) Uani 1 1 d . . . . .
Ge1 Ge 0.55551(3) 0.04714(3) 0.76673(3) 0.02117(10) Uani 1 1 d . . . . .
N1 N 0.6013(2) -0.0643(2) 0.6755(2) 0.0234(5) Uani 1 1 d . . . . .
N2 N 0.5992(2) -0.0602(2) 0.8792(2) 0.0238(5) Uani 1 1 d . . . . .
P1 P 0.78160(7) 0.19238(6) 0.65355(6) 0.02219(16) Uani 1 1 d . . . . .
P2 P 0.78788(7) 0.19238(7) 1.01262(6) 0.02466(16) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C3 1.532(5) . ?
C2 C3 1.517(5) . ?
C3 P1 1.847(3) . ?
C4 C6 1.528(5) . ?
C5 C6 1.525(5) . ?
C6 P1 1.846(3) . ?
C7 C8 1.501(4) . ?
C7 P1 1.848(3) . ?
C8 C9 1.371(4) . ?
C8 N1 1.385(4) . ?
C9 C10 1.423(5) . ?
C10 C11 1.369(4) . ?
C11 N1 1.390(4) . ?
C11 C12 1.518(4) . ?
C12 C15 1.516(4) . ?
C12 C14 1.535(4) . ?
C12 C13 1.543(5) . ?
C15 C16 1.367(4) . ?
C15 N2 1.388(4) . ?
C16 C17 1.419(5) . ?
C17 C18 1.370(4) . ?
C18 N2 1.388(4) . ?
C18 C19 1.499(4) . ?
C19 P2 1.848(3) . ?
C20 C22 1.521(5) . ?
C20 C21 1.533(5) . ?
C20 P2 1.848(3) . ?
C23 C25 1.527(5) . ?
C23 C24 1.531(5) . ?
C23 P2 1.841(4) . ?
C26 Cl2 1.684(8) . ?
C26 Cl3 1.703(8) . ?
Ag1 P2 2.4054(12) . ?
Ag1 P1 2.4084(12) . ?
Ag1 Ge1 2.7155(10) . ?
Cl1 Ge1 2.3230(13) . ?
Ge1 N2 1.921(2) . ?
Ge1 N1 1.932(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C3 C1 112.4(3) . . ?
C2 C3 P1 114.4(2) . . ?
C1 C3 P1 111.6(3) . . ?
C5 C6 C4 110.7(3) . . ?
C5 C6 P1 109.9(2) . . ?
C4 C6 P1 110.1(2) . . ?
C8 C7 P1 112.6(2) . . ?
C9 C8 N1 109.0(3) . . ?
C9 C8 C7 128.3(3) . . ?
N1 C8 C7 122.7(3) . . ?
C8 C9 C10 106.9(3) . . ?
C11 C10 C9 107.9(3) . . ?
C10 C11 N1 108.4(3) . . ?
C10 C11 C12 130.2(3) . . ?
N1 C11 C12 121.4(3) . . ?
C15 C12 C11 110.6(2) . . ?
C15 C12 C14 109.1(3) . . ?
C11 C12 C14 108.7(3) . . ?
C15 C12 C13 111.0(3) . . ?
C11 C12 C13 110.5(3) . . ?
C14 C12 C13 106.8(3) . . ?
C16 C15 N2 108.7(3) . . ?
C16 C15 C12 129.2(3) . . ?
N2 C15 C12 122.1(3) . . ?
C15 C16 C17 107.7(3) . . ?
C18 C17 C16 107.2(3) . . ?
C17 C18 N2 108.8(3) . . ?
C17 C18 C19 128.1(3) . . ?
N2 C18 C19 123.1(3) . . ?
C18 C19 P2 113.6(2) . . ?
C22 C20 C21 112.3(3) . . ?
C22 C20 P2 114.1(3) . . ?
C21 C20 P2 112.3(3) . . ?
C25 C23 C24 110.5(3) . . ?
C25 C23 P2 111.1(3) . . ?
C24 C23 P2 109.7(3) . . ?
Cl2 C26 Cl3 113.0(4) . . ?
P2 Ag1 P1 173.49(3) . . ?
P2 Ag1 Ge1 93.54(2) . . ?
P1 Ag1 Ge1 92.30(2) . . ?
N2 Ge1 N1 90.86(11) . . ?
N2 Ge1 Cl1 101.49(8) . . ?
N1 Ge1 Cl1 99.61(8) . . ?
N2 Ge1 Ag1 98.85(8) . . ?
N1 Ge1 Ag1 98.99(8) . . ?
Cl1 Ge1 Ag1 152.09(3) . . ?
C8 N1 C11 107.8(2) . . ?
C8 N1 Ge1 122.7(2) . . ?
C11 N1 Ge1 127.8(2) . . ?
C18 N2 C15 107.6(2) . . ?
C18 N2 Ge1 123.5(2) . . ?
C15 N2 Ge1 128.1(2) . . ?
C6 P1 C3 107.79(15) . . ?
C6 P1 C7 105.04(14) . . ?
C3 P1 C7 103.21(15) . . ?
C6 P1 Ag1 112.70(11) . . ?
C3 P1 Ag1 117.71(11) . . ?
C7 P1 Ag1 109.28(10) . . ?
C23 P2 C20 108.22(17) . . ?
C23 P2 C19 104.34(15) . . ?
C20 P2 C19 103.21(15) . . ?
C23 P2 Ag1 112.23(12) . . ?
C20 P2 Ag1 119.33(12) . . ?
C19 P2 Ag1 108.12(10) . . ?

_refine_diff_density_max         1.212
_refine_diff_density_min         -1.616
_refine_diff_density_rms         0.089

_shelxl_version_number           2014-3

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

data_4
_database_code_depnum_ccdc_archive 'CCDC 1937811'
loop_
_audit_author_name
_audit_author_address
'Javier A. Cabeza'
;University of Oviedo
Spain
;
_audit_update_record             
;
2019-07-02 deposited with the CCDC.	2019-07-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H42 Au Cl Ge N2 P2, C H2 Cl2'
_chemical_formula_sum            'C26 H44 Au Cl3 Ge N2 P2'
_chemical_formula_weight         822.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   11.1202(9)
_cell_length_b                   11.3734(9)
_cell_length_c                   13.3691(11)
_cell_angle_alpha                91.388(4)
_cell_angle_beta                 109.574(4)
_cell_angle_gamma                92.995(4)
_cell_volume                     1589.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1994
_cell_measurement_theta_min      3,59
_cell_measurement_theta_max      35,85

_exptl_crystal_description       PLATE
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_F_000             812
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    5.927
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6889
_exptl_absorpt_correction_T_max  0.7909
_exptl_absorpt_process_details   
; 
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction 

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

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON III-14'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            203662
_diffrn_reflns_av_unetI/netI     0.0087
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_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         2.363
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6247
_reflns_number_gt                6182
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

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

_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)+(0.0410P)²+4.4251P] 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         6247
_refine_ls_number_parameters     326
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0235
_refine_ls_wR_factor_ref         0.0742
_refine_ls_wR_factor_gt          0.0683
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_restrained_S_all      1.184
_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
C1 C 0.4513(4) 0.3493(5) -0.0758(4) 0.0348(10) Uani 1 1 d . . . . .
H1A H 0.3819 0.3901 -0.1255 0.052 Uiso 1 1 calc R U . . .
H1B H 0.4656 0.3792 -0.0031 0.052 Uiso 1 1 calc R U . . .
H1C H 0.4280 0.2645 -0.0817 0.052 Uiso 1 1 calc R U . . .
C2 C 0.5535(4) 0.3359(4) -0.2185(3) 0.0306(9) Uani 1 1 d . . . . .
H2A H 0.5373 0.2502 -0.2293 0.046 Uiso 1 1 calc R U . . .
H2B H 0.6305 0.3601 -0.2349 0.046 Uiso 1 1 calc R U . . .
H2C H 0.4802 0.3746 -0.2655 0.046 Uiso 1 1 calc R U . . .
C3 C 0.5729(4) 0.3715(4) -0.1025(3) 0.0245(8) Uani 1 1 d . . . . .
H3 H 0.5914 0.4589 -0.0958 0.029 Uiso 1 1 calc R U . . .
C4 C 0.6180(5) 0.0752(4) -0.0531(4) 0.0365(11) Uani 1 1 d . . . . .
H4A H 0.6302 -0.0043 -0.0764 0.055 Uiso 1 1 calc R U . . .
H4B H 0.5376 0.1023 -0.1011 0.055 Uiso 1 1 calc R U . . .
H4C H 0.6148 0.0739 0.0192 0.055 Uiso 1 1 calc R U . . .
C5 C 0.8582(5) 0.1144(4) 0.0137(4) 0.0334(10) Uani 1 1 d . . . . .
H5A H 0.8634 0.1164 0.0884 0.050 Uiso 1 1 calc R U . . .
H5B H 0.9286 0.1647 0.0060 0.050 Uiso 1 1 calc R U . . .
H5C H 0.8643 0.0333 -0.0097 0.050 Uiso 1 1 calc R U . . .
C6 C 0.7300(4) 0.1596(3) -0.0547(3) 0.0229(8) Uani 1 1 d . . . . .
H6 H 0.7291 0.1631 -0.1296 0.028 Uiso 1 1 calc R U . . .
C7 C 0.8500(3) 0.3974(3) -0.0230(3) 0.0159(7) Uani 1 1 d . . . . .
H7A H 0.9305 0.3617 0.0170 0.019 Uiso 1 1 calc R U . . .
H7B H 0.8422 0.3949 -0.0990 0.019 Uiso 1 1 calc R U . . .
C8 C 0.8575(3) 0.5234(3) 0.0152(3) 0.0154(7) Uani 1 1 d . . . . .
C9 C 0.8184(3) 0.6199(3) -0.0443(3) 0.0178(7) Uani 1 1 d . . . . .
H9 H 0.7828 0.6202 -0.1196 0.021 Uiso 1 1 calc R U . . .
C10 C 0.8410(4) 0.7191(3) 0.0275(3) 0.0187(7) Uani 1 1 d . . . . .
H10 H 0.8235 0.7980 0.0091 0.022 Uiso 1 1 calc R U . . .
C11 C 0.8929(4) 0.6801(3) 0.1286(3) 0.0165(7) Uani 1 1 d . . . . .
C12 C 0.9313(4) 0.7489(3) 0.2343(3) 0.0189(7) Uani 1 1 d . . . . .
C13 C 1.0773(4) 0.7778(4) 0.2788(3) 0.0255(8) Uani 1 1 d . . . . .
H13A H 1.1213 0.7043 0.2916 0.038 Uiso 1 1 calc R U . . .
H13B H 1.0993 0.8247 0.3456 0.038 Uiso 1 1 calc R U . . .
H13C H 1.1040 0.8227 0.2272 0.038 Uiso 1 1 calc R U . . .
C14 C 0.8678(5) 0.8667(3) 0.2172(3) 0.0281(9) Uani 1 1 d . . . . .
H14A H 0.8961 0.9116 0.1665 0.042 Uiso 1 1 calc R U . . .
H14B H 0.8920 0.9120 0.2851 0.042 Uiso 1 1 calc R U . . .
H14C H 0.7746 0.8519 0.1890 0.042 Uiso 1 1 calc R U . . .
C15 C 0.8865(4) 0.6806(3) 0.3128(3) 0.0167(7) Uani 1 1 d . . . . .
C16 C 0.8248(4) 0.7183(3) 0.3800(3) 0.0197(7) Uani 1 1 d . . . . .
H16 H 0.8009 0.7962 0.3873 0.024 Uiso 1 1 calc R U . . .
C17 C 0.8031(4) 0.6198(3) 0.4366(3) 0.0180(7) Uani 1 1 d . . . . .
H17 H 0.7621 0.6196 0.4885 0.022 Uiso 1 1 calc R U . . .
C18 C 0.8527(3) 0.5251(3) 0.4022(3) 0.0153(7) Uani 1 1 d . . . . .
C19 C 0.8525(3) 0.4001(3) 0.4349(3) 0.0154(7) Uani 1 1 d . . . . .
H19A H 0.8452 0.3985 0.5066 0.019 Uiso 1 1 calc R U . . .
H19B H 0.9348 0.3677 0.4389 0.019 Uiso 1 1 calc R U . . .
C20 C 0.5769(4) 0.3642(4) 0.3602(3) 0.0225(8) Uani 1 1 d . . . . .
H20 H 0.5888 0.4519 0.3595 0.027 Uiso 1 1 calc R U . . .
C21 C 0.5636(4) 0.3384(5) 0.4675(4) 0.0314(10) Uani 1 1 d . . . . .
H21A H 0.4911 0.3787 0.4751 0.047 Uiso 1 1 calc R U . . .
H21B H 0.6421 0.3667 0.5246 0.047 Uiso 1 1 calc R U . . .
H21C H 0.5489 0.2533 0.4720 0.047 Uiso 1 1 calc R U . . .
C22 C 0.4557(4) 0.3293(5) 0.2685(4) 0.0365(11) Uani 1 1 d . . . . .
H22A H 0.4353 0.2444 0.2685 0.055 Uiso 1 1 calc R U . . .
H22B H 0.4682 0.3484 0.2014 0.055 Uiso 1 1 calc R U . . .
H22C H 0.3852 0.3725 0.2762 0.055 Uiso 1 1 calc R U . . .
C23 C 0.7398(4) 0.1570(3) 0.3927(3) 0.0204(8) Uani 1 1 d . . . . .
H23 H 0.7260 0.1579 0.4628 0.025 Uiso 1 1 calc R U . . .
C24 C 0.8754(4) 0.1208(4) 0.4097(4) 0.0265(9) Uani 1 1 d . . . . .
H24A H 0.8831 0.0396 0.4327 0.040 Uiso 1 1 calc R U . . .
H24B H 0.9368 0.1735 0.4643 0.040 Uiso 1 1 calc R U . . .
H24C H 0.8934 0.1262 0.3430 0.040 Uiso 1 1 calc R U . . .
C25 C 0.6407(5) 0.0689(4) 0.3170(5) 0.0426(13) Uani 1 1 d . . . . .
H25A H 0.6522 0.0675 0.2474 0.064 Uiso 1 1 calc R U . . .
H25B H 0.5546 0.0924 0.3092 0.064 Uiso 1 1 calc R U . . .
H25C H 0.6517 -0.0098 0.3457 0.064 Uiso 1 1 calc R U . . .
C26 C 0.8044(9) 0.8368(8) 0.6606(9) 0.088(3) Uani 1 1 d . . . . .
H26A H 0.8863 0.8353 0.6465 0.106 Uiso 1 1 calc R U . . .
H26B H 0.7672 0.7548 0.6535 0.106 Uiso 1 1 calc R U . . .
Au1 Au 0.72543(2) 0.31239(2) 0.16953(2) 0.01671(6) Uani 1 1 d . . . . .
Cl1 Cl 1.17519(8) 0.48817(8) 0.30143(7) 0.01987(18) Uani 1 1 d . . . . .
Cl2 Cl 0.8340(3) 0.8915(2) 0.78875(17) 0.1239(13) Uani 1 1 d . . . . .
Cl3 Cl 0.7038(3) 0.9179(2) 0.56968(17) 0.1172(11) Uani 1 1 d . . . . .
Ge1 Ge 0.95168(3) 0.45085(3) 0.23532(3) 0.01341(9) Uani 1 1 d . . . . .
N1 N 0.9051(3) 0.5596(3) 0.1221(2) 0.0143(6) Uani 1 1 d . . . . .
N2 N 0.9044(3) 0.5614(3) 0.3259(2) 0.0149(6) Uani 1 1 d . . . . .
P1 P 0.71455(9) 0.30910(9) -0.00727(7) 0.01656(19) Uani 1 1 d . . . . .
P2 P 0.72040(9) 0.30650(8) 0.34184(7) 0.01441(18) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C3 1.520(6) . ?
C2 C3 1.533(6) . ?
C3 P1 1.850(4) . ?
C4 C6 1.539(6) . ?
C5 C6 1.536(6) . ?
C6 P1 1.837(4) . ?
C7 C8 1.498(5) . ?
C7 P1 1.840(4) . ?
C8 C9 1.374(5) . ?
C8 N1 1.391(5) . ?
C9 C10 1.419(5) . ?
C10 C11 1.374(5) . ?
C11 N1 1.387(5) . ?
C11 C12 1.517(5) . ?
C12 C15 1.517(5) . ?
C12 C14 1.533(5) . ?
C12 C13 1.545(6) . ?
C15 C16 1.375(5) . ?
C15 N2 1.387(5) . ?
C16 C17 1.421(5) . ?
C17 C18 1.373(5) . ?
C18 N2 1.389(5) . ?
C18 C19 1.497(5) . ?
C19 P2 1.840(4) . ?
C20 C22 1.513(6) . ?
C20 C21 1.525(6) . ?
C20 P2 1.844(4) . ?
C23 C25 1.527(6) . ?
C23 C24 1.528(6) . ?
C23 P2 1.842(4) . ?
C26 Cl3 1.683(10) . ?
C26 Cl2 1.727(11) . ?
Au1 P1 2.3253(10) . ?
Au1 P2 2.3254(9) . ?
Au1 Ge1 2.7604(4) . ?
Cl1 Ge1 2.3534(9) . ?
Ge1 N1 1.929(3) . ?
Ge1 N2 1.935(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 C3 C2 112.0(4) . . ?
C1 C3 P1 113.5(3) . . ?
C2 C3 P1 113.0(3) . . ?
C5 C6 C4 110.6(4) . . ?
C5 C6 P1 109.7(3) . . ?
C4 C6 P1 111.2(3) . . ?
C8 C7 P1 113.1(2) . . ?
C9 C8 N1 108.9(3) . . ?
C9 C8 C7 128.1(3) . . ?
N1 C8 C7 123.1(3) . . ?
C8 C9 C10 107.2(3) . . ?
C11 C10 C9 107.6(3) . . ?
C10 C11 N1 108.7(3) . . ?
C10 C11 C12 129.2(3) . . ?
N1 C11 C12 122.1(3) . . ?
C11 C12 C15 110.1(3) . . ?
C11 C12 C14 108.8(3) . . ?
C15 C12 C14 108.9(3) . . ?
C11 C12 C13 111.0(3) . . ?
C15 C12 C13 110.8(3) . . ?
C14 C12 C13 107.1(3) . . ?
C16 C15 N2 108.5(3) . . ?
C16 C15 C12 129.7(3) . . ?
N2 C15 C12 121.8(3) . . ?
C15 C16 C17 107.7(3) . . ?
C18 C17 C16 107.2(3) . . ?
C17 C18 N2 108.8(3) . . ?
C17 C18 C19 128.7(3) . . ?
N2 C18 C19 122.4(3) . . ?
C18 C19 P2 112.3(2) . . ?
C22 C20 C21 112.3(4) . . ?
C22 C20 P2 112.8(3) . . ?
C21 C20 P2 113.8(3) . . ?
C25 C23 C24 110.9(4) . . ?
C25 C23 P2 110.6(3) . . ?
C24 C23 P2 110.3(3) . . ?
Cl3 C26 Cl2 112.2(5) . . ?
P1 Au1 P2 175.30(3) . . ?
P1 Au1 Ge1 92.75(2) . . ?
P2 Au1 Ge1 91.95(2) . . ?
N1 Ge1 N2 89.76(13) . . ?
N1 Ge1 Cl1 100.74(9) . . ?
N2 Ge1 Cl1 99.44(9) . . ?
N1 Ge1 Au1 97.05(9) . . ?
N2 Ge1 Au1 97.11(9) . . ?
Cl1 Ge1 Au1 155.66(3) . . ?
C11 N1 C8 107.6(3) . . ?
C11 N1 Ge1 128.7(2) . . ?
C8 N1 Ge1 123.0(2) . . ?
C15 N2 C18 107.8(3) . . ?
C15 N2 Ge1 128.3(2) . . ?
C18 N2 Ge1 122.4(2) . . ?
C6 P1 C7 104.60(18) . . ?
C6 P1 C3 109.21(19) . . ?
C7 P1 C3 103.58(18) . . ?
C6 P1 Au1 111.19(14) . . ?
C7 P1 Au1 110.92(12) . . ?
C3 P1 Au1 116.45(14) . . ?
C19 P2 C23 105.75(17) . . ?
C19 P2 C20 103.35(18) . . ?
C23 P2 C20 108.84(19) . . ?
C19 P2 Au1 111.27(12) . . ?
C23 P2 Au1 111.99(13) . . ?
C20 P2 Au1 114.92(13) . . ?

_refine_diff_density_max         1.784
_refine_diff_density_min         -2.223
_refine_diff_density_rms         0.237

_shelxl_version_number           2014-3

