# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_compound_1a
_database_code_depnum_ccdc_archive 'CCDC 2057295'
loop_
_audit_author_name
_audit_author_address
'Terrance Hadlington'
;TU Munich
Germany
;
_audit_update_record             
;
2021-01-19 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H39 Cl Ge N P Si'
_chemical_formula_sum            'C37 H39 Cl Ge N P Si'
_chemical_formula_weight         664.79

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

_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                   11.000(2)
_cell_length_b                   12.100(2)
_cell_length_c                   13.500(3)
_cell_angle_alpha                96.00(3)
_cell_angle_beta                 93.00(3)
_cell_angle_gamma                109.00(3)
_cell_volume                     1682.5(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2000
_cell_measurement_theta_min      1.92
_cell_measurement_theta_max      32.50

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    1.099
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.876
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_process_details   'STOE X-AREA 1.76'

_diffrn_ambient_temperature      150(2)
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            16730
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.047
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6600
_reflns_number_gt                5791
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0525P)²+0.5403P] 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         6600
_refine_ls_number_parameters     383
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0318
_refine_ls_wR_factor_ref         0.0855
_refine_ls_wR_factor_gt          0.0805
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_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
Ge1 Ge 0.49753(2) 0.58821(2) 0.11920(2) 0.02329(7) Uani 1 1 d . . . . .
Cl1 Cl 0.27630(5) 0.50889(4) 0.13601(4) 0.03137(12) Uani 1 1 d . . . . .
P1 P 0.52140(5) 0.43512(4) 0.21676(4) 0.02279(11) Uani 1 1 d . . . . .
Si1 Si 0.54160(5) 0.65414(4) 0.36147(4) 0.02160(12) Uani 1 1 d . . . . .
N1 N 0.55751(15) 0.69304(13) 0.24231(12) 0.0221(3) Uani 1 1 d . . . . .
C1 C 0.62147(18) 0.81358(16) 0.22633(14) 0.0235(4) Uani 1 1 d . . . . .
C32 C 0.68370(19) 0.42850(17) 0.21814(15) 0.0264(4) Uani 1 1 d . . . . .
C6 C 0.75433(19) 0.85234(18) 0.21272(14) 0.0273(4) Uani 1 1 d . . . . .
C13 C 0.41021(19) 0.69371(17) 0.42642(14) 0.0255(4) Uani 1 1 d . . . . .
C19 C 0.69482(18) 0.72588(18) 0.44621(14) 0.0270(4) Uani 1 1 d . . . . .
C26 C 0.41125(19) 0.28715(17) 0.17594(15) 0.0266(4) Uani 1 1 d . . . . .
C25 C 0.49334(19) 0.48677(16) 0.34172(14) 0.0253(4) Uani 1 1 d . . . . .
H25A H 0.544067 0.461075 0.391671 0.030 Uiso 1 1 calc R U . . .
H25B H 0.400797 0.451570 0.351732 0.030 Uiso 1 1 calc R U . . .
C2 C 0.5497(2) 0.89185(17) 0.22075(14) 0.0273(4) Uani 1 1 d . . . . .
C33 C 0.7469(2) 0.4484(2) 0.13135(17) 0.0355(5) Uani 1 1 d . . . . .
H33 H 0.705606 0.466743 0.074848 0.043 Uiso 1 1 calc R U . . .
C10 C 0.83337(19) 0.76929(19) 0.20527(16) 0.0303(4) Uani 1 1 d . . . . .
H10 H 0.778681 0.691699 0.223507 0.036 Uiso 1 1 calc R U . . .
C7 C 0.4038(2) 0.84970(19) 0.22287(16) 0.0313(4) Uani 1 1 d . . . . .
H7 H 0.378519 0.773288 0.251493 0.038 Uiso 1 1 calc R U . . .
C5 C 0.8136(2) 0.97001(19) 0.20027(16) 0.0334(5) Uani 1 1 d . . . . .
H5 H 0.903489 0.997525 0.192491 0.040 Uiso 1 1 calc R U . . .
C37 C 0.7464(2) 0.4024(2) 0.29979(17) 0.0367(5) Uani 1 1 d . . . . .
H37 H 0.704006 0.387290 0.358960 0.044 Uiso 1 1 calc R U . . .
C24 C 0.7451(2) 0.8495(2) 0.46877(16) 0.0332(5) Uani 1 1 d . . . . .
H24 H 0.703955 0.896243 0.437196 0.040 Uiso 1 1 calc R U . . .
C20 C 0.7603(2) 0.6612(2) 0.49320(16) 0.0344(5) Uani 1 1 d . . . . .
H20 H 0.729608 0.577625 0.479564 0.041 Uiso 1 1 calc R U . . .
C3 C 0.6144(2) 1.00838(19) 0.20729(16) 0.0331(5) Uani 1 1 d . . . . .
H3 H 0.567236 1.061386 0.203833 0.040 Uiso 1 1 calc R U . . .
C27 C 0.4389(2) 0.22135(18) 0.09419(15) 0.0314(4) Uani 1 1 d . . . . .
H27 H 0.520922 0.248569 0.068770 0.038 Uiso 1 1 calc R U . . .
C14 C 0.2801(2) 0.6378(2) 0.39021(16) 0.0322(5) Uani 1 1 d . . . . .
H14 H 0.257906 0.573492 0.338228 0.039 Uiso 1 1 calc R U . . .
C18 C 0.4376(2) 0.78593(19) 0.50561(16) 0.0326(5) Uani 1 1 d . . . . .
H18 H 0.524153 0.823093 0.534038 0.039 Uiso 1 1 calc R U . . .
C4 C 0.7455(2) 1.04826(18) 0.19888(17) 0.0362(5) Uani 1 1 d . . . . .
H4 H 0.788834 1.128653 0.192199 0.043 Uiso 1 1 calc R U . . .
C8 C 0.3567(2) 0.9358(2) 0.28986(18) 0.0389(5) Uani 1 1 d . . . . .
H8A H 0.401217 0.950474 0.357180 0.058 Uiso 1 1 calc R U . . .
H8B H 0.263393 0.901281 0.293487 0.058 Uiso 1 1 calc R U . . .
H8C H 0.375498 1.010231 0.261512 0.058 Uiso 1 1 calc R U . . .
C17 C 0.3402(2) 0.8239(2) 0.54325(18) 0.0418(6) Uani 1 1 d . . . . .
H17 H 0.361123 0.887754 0.595631 0.050 Uiso 1 1 calc R U . . .
C23 C 0.8533(2) 0.9048(2) 0.53612(17) 0.0417(6) Uani 1 1 d . . . . .
H23 H 0.884034 0.988236 0.551046 0.050 Uiso 1 1 calc R U . . .
C34 C 0.8701(2) 0.4414(2) 0.1276(2) 0.0446(6) Uani 1 1 d . . . . .
H34 H 0.912013 0.453245 0.067868 0.054 Uiso 1 1 calc R U . . .
C15 C 0.1832(2) 0.6748(2) 0.42886(17) 0.0381(5) Uani 1 1 d . . . . .
H15 H 0.095719 0.635450 0.403450 0.046 Uiso 1 1 calc R U . . .
C16 C 0.2136(2) 0.7689(2) 0.50449(19) 0.0419(6) Uani 1 1 d . . . . .
H16 H 0.147468 0.795476 0.529527 0.050 Uiso 1 1 calc R U . . .
C35 C 0.9322(2) 0.4173(2) 0.2098(2) 0.0479(6) Uani 1 1 d . . . . .
H35 H 1.017076 0.413971 0.207400 0.057 Uiso 1 1 calc R U . . .
C12 C 0.8654(2) 0.7489(2) 0.09709(18) 0.0392(5) Uani 1 1 d . . . . .
H12A H 0.785144 0.714437 0.053063 0.059 Uiso 1 1 calc R U . . .
H12B H 0.915437 0.695049 0.092751 0.059 Uiso 1 1 calc R U . . .
H12C H 0.916146 0.824335 0.076339 0.059 Uiso 1 1 calc R U . . .
C22 C 0.9162(2) 0.8392(3) 0.58124(18) 0.0492(7) Uani 1 1 d . . . . .
H22 H 0.990725 0.877173 0.626722 0.059 Uiso 1 1 calc R U . . .
C21 C 0.8700(2) 0.7172(3) 0.55980(18) 0.0466(6) Uani 1 1 d . . . . .
H21 H 0.913250 0.671611 0.590628 0.056 Uiso 1 1 calc R U . . .
C29 C 0.2296(2) 0.0754(2) 0.08724(19) 0.0419(6) Uani 1 1 d . . . . .
H29 H 0.166602 0.004071 0.056544 0.050 Uiso 1 1 calc R U . . .
C28 C 0.3476(2) 0.11670(19) 0.04995(17) 0.0381(5) Uani 1 1 d . . . . .
H28 H 0.366634 0.073345 -0.006392 0.046 Uiso 1 1 calc R U . . .
C31 C 0.2935(2) 0.2446(2) 0.21431(19) 0.0407(5) Uani 1 1 d . . . . .
H31 H 0.273934 0.287276 0.270821 0.049 Uiso 1 1 calc R U . . .
C9 C 0.3375(2) 0.8253(2) 0.11620(18) 0.0392(5) Uani 1 1 d . . . . .
H9A H 0.367362 0.896754 0.083544 0.059 Uiso 1 1 calc R U . . .
H9B H 0.243752 0.801728 0.118773 0.059 Uiso 1 1 calc R U . . .
H9C H 0.359052 0.761705 0.078152 0.059 Uiso 1 1 calc R U . . .
C11 C 0.9574(2) 0.8132(2) 0.27649(18) 0.0414(5) Uani 1 1 d . . . . .
H11A H 1.015520 0.886553 0.257264 0.062 Uiso 1 1 calc R U . . .
H11B H 0.999996 0.753431 0.272614 0.062 Uiso 1 1 calc R U . . .
H11C H 0.935896 0.827602 0.345108 0.062 Uiso 1 1 calc R U . . .
C36 C 0.8700(2) 0.3981(3) 0.2955(2) 0.0491(6) Uani 1 1 d . . . . .
H36 H 0.912588 0.381746 0.352376 0.059 Uiso 1 1 calc R U . . .
C30 C 0.2033(2) 0.1384(2) 0.1696(2) 0.0474(6) Uani 1 1 d . . . . .
H30 H 0.122459 0.108955 0.196305 0.057 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N1 1.9251(17) . ?
Ge1 Cl1 2.3403(8) . ?
Ge1 P1 2.4546(8) . ?
P1 C32 1.812(2) . ?
P1 C26 1.814(2) . ?
P1 C25 1.814(2) . ?
Si1 N1 1.7246(17) . ?
Si1 C19 1.882(2) . ?
Si1 C13 1.893(2) . ?
Si1 C25 1.904(2) . ?
N1 C1 1.443(2) . ?
C1 C6 1.411(3) . ?
C1 C2 1.422(3) . ?
C32 C37 1.388(3) . ?
C32 C33 1.396(3) . ?
C6 C5 1.392(3) . ?
C6 C10 1.527(3) . ?
C13 C14 1.405(3) . ?
C13 C18 1.406(3) . ?
C19 C20 1.399(3) . ?
C19 C24 1.409(3) . ?
C26 C31 1.380(3) . ?
C26 C27 1.398(3) . ?
C2 C3 1.393(3) . ?
C2 C7 1.520(3) . ?
C33 C34 1.389(3) . ?
C10 C11 1.534(3) . ?
C10 C12 1.534(3) . ?
C7 C9 1.534(3) . ?
C7 C8 1.541(3) . ?
C5 C4 1.386(3) . ?
C37 C36 1.381(3) . ?
C24 C23 1.390(3) . ?
C20 C21 1.397(3) . ?
C3 C4 1.379(3) . ?
C27 C28 1.386(3) . ?
C14 C15 1.389(3) . ?
C18 C17 1.395(3) . ?
C17 C16 1.380(4) . ?
C23 C22 1.376(4) . ?
C34 C35 1.379(4) . ?
C15 C16 1.387(4) . ?
C35 C36 1.377(4) . ?
C22 C21 1.389(4) . ?
C29 C28 1.374(4) . ?
C29 C30 1.378(4) . ?
C31 C30 1.394(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
N1 Ge1 Cl1 101.45(6) . . ?
N1 Ge1 P1 85.38(5) . . ?
Cl1 Ge1 P1 86.08(3) . . ?
C32 P1 C26 107.15(9) . . ?
C32 P1 C25 109.28(10) . . ?
C26 P1 C25 110.61(10) . . ?
C32 P1 Ge1 111.31(7) . . ?
C26 P1 Ge1 115.63(7) . . ?
C25 P1 Ge1 102.74(7) . . ?
N1 Si1 C19 112.15(9) . . ?
N1 Si1 C13 114.16(8) . . ?
C19 Si1 C13 106.29(9) . . ?
N1 Si1 C25 103.92(9) . . ?
C19 Si1 C25 112.56(10) . . ?
C13 Si1 C25 107.82(9) . . ?
C1 N1 Si1 121.04(13) . . ?
C1 N1 Ge1 112.73(12) . . ?
Si1 N1 Ge1 126.23(9) . . ?
C6 C1 C2 120.11(18) . . ?
C6 C1 N1 119.82(17) . . ?
C2 C1 N1 120.02(17) . . ?
C37 C32 C33 118.85(19) . . ?
C37 C32 P1 123.41(16) . . ?
C33 C32 P1 117.73(16) . . ?
C5 C6 C1 118.26(19) . . ?
C5 C6 C10 118.91(18) . . ?
C1 C6 C10 122.74(18) . . ?
C14 C13 C18 117.17(19) . . ?
C14 C13 Si1 120.19(15) . . ?
C18 C13 Si1 122.38(16) . . ?
C20 C19 C24 117.0(2) . . ?
C20 C19 Si1 122.73(17) . . ?
C24 C19 Si1 120.23(16) . . ?
C31 C26 C27 119.16(19) . . ?
C31 C26 P1 121.61(16) . . ?
C27 C26 P1 118.63(15) . . ?
P1 C25 Si1 110.85(10) . . ?
C3 C2 C1 118.80(19) . . ?
C3 C2 C7 119.46(19) . . ?
C1 C2 C7 121.63(18) . . ?
C34 C33 C32 120.0(2) . . ?
C6 C10 C11 113.18(18) . . ?
C6 C10 C12 109.92(18) . . ?
C11 C10 C12 110.22(18) . . ?
C2 C7 C9 110.28(18) . . ?
C2 C7 C8 112.76(18) . . ?
C9 C7 C8 111.20(18) . . ?
C4 C5 C6 122.0(2) . . ?
C36 C37 C32 120.4(2) . . ?
C23 C24 C19 121.6(2) . . ?
C21 C20 C19 121.2(2) . . ?
C4 C3 C2 121.3(2) . . ?
C28 C27 C26 120.5(2) . . ?
C15 C14 C13 121.3(2) . . ?
C17 C18 C13 121.3(2) . . ?
C3 C4 C5 119.4(2) . . ?
C16 C17 C18 120.1(2) . . ?
C22 C23 C24 120.3(2) . . ?
C35 C34 C33 120.5(2) . . ?
C16 C15 C14 120.2(2) . . ?
C17 C16 C15 119.9(2) . . ?
C36 C35 C34 119.4(2) . . ?
C23 C22 C21 119.5(2) . . ?
C22 C21 C20 120.4(2) . . ?
C28 C29 C30 119.4(2) . . ?
C29 C28 C27 120.3(2) . . ?
C26 C31 C30 119.5(2) . . ?
C35 C36 C37 120.8(2) . . ?
C29 C30 C31 121.1(2) . . ?

_refine_diff_density_max         0.515
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.062


####################################################################### 
# 
# 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_compound_3a
_database_code_depnum_ccdc_archive 'CCDC 2057300'
loop_
_audit_author_name
_audit_author_address
'Terrance Hadlington'
;TU Munich
Germany
;
_audit_update_record             
;
2021-01-19 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C43 H45 Br Ge N P Si'
_chemical_formula_sum            'C43 H45 Br Ge N P Si'

_chemical_formula_weight         787.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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                   11.330(2)
_cell_length_b                   13.510(3)
_cell_length_c                   13.610(3)
_cell_angle_alpha                79.10(3)
_cell_angle_beta                 86.70(3)
_cell_angle_gamma                69.60(3)
_cell_volume                     1917.3(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2000
_cell_measurement_theta_min      1.92
_cell_measurement_theta_max      32.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    1.945
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.698
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'STOE X-AREA 1.76'

_diffrn_ambient_temperature      150(2)
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            16584
_diffrn_reflns_av_unetI/netI     0.0742
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.918
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.983
_reflns_number_total             7387
_reflns_number_gt                5314
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0817P)²+4.2187P] 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         7387
_refine_ls_number_parameters     437
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0513
_refine_ls_wR_factor_ref         0.1598
_refine_ls_wR_factor_gt          0.1293
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_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
Ge1 Ge 0.58149(5) 0.43757(4) 0.39119(3) 0.01807(15) Uani 1 1 d . . . . .
Br1 Br 0.71703(5) 0.54668(4) 0.32150(4) 0.02668(16) Uani 1 1 d . . . . .
P3 P 0.42643(11) 0.56210(10) 0.26585(9) 0.0167(3) Uani 1 1 d . . . . .
Si1 Si 0.58547(12) 0.37085(10) 0.17319(9) 0.0168(3) Uani 1 1 d . . . . .
N1 N 0.6103(4) 0.3387(3) 0.3012(3) 0.0154(8) Uani 1 1 d . . . . .
C32 C 0.3863(4) 0.7062(4) 0.2540(3) 0.0179(10) Uani 1 1 d . . . . .
C7 C 0.8851(5) 0.2292(4) 0.3417(4) 0.0222(10) Uani 1 1 d . . . . .
H7 H 0.842264 0.301792 0.300912 0.027 Uiso 1 1 calc R U . . .
C19 C 0.4945(5) 0.2958(4) 0.1250(3) 0.0196(10) Uani 1 1 d . . . . .
C26 C 0.2795(5) 0.5356(4) 0.2875(4) 0.0213(10) Uani 1 1 d . . . . .
C31 C 0.2486(5) 0.5057(4) 0.3858(4) 0.0250(11) Uani 1 1 d . . . . .
H31 H 0.302808 0.500738 0.438630 0.030 Uiso 1 1 calc R U . . .
C2 C 0.7903(5) 0.1705(4) 0.3608(3) 0.0201(10) Uani 1 1 d . . . . .
C23 C 0.3178(6) 0.2951(5) 0.0291(4) 0.0346(13) Uani 1 1 d . . . . .
H23 H 0.242657 0.333716 -0.008906 0.042 Uiso 1 1 calc R U . . .
C1 C 0.6592(5) 0.2257(4) 0.3492(3) 0.0186(10) Uani 1 1 d . . . . .
C34 C 0.3720(6) 0.8810(4) 0.1612(4) 0.0341(13) Uani 1 1 d . . . . .
H34 H 0.383757 0.924822 0.100774 0.041 Uiso 1 1 calc R U . . .
C3 C 0.8332(5) 0.0609(4) 0.3980(4) 0.0268(11) Uani 1 1 d . . . . .
H3 H 0.921118 0.023299 0.406800 0.032 Uiso 1 1 calc R U . . .
C27 C 0.1996(5) 0.5432(4) 0.2102(4) 0.0257(11) Uani 1 1 d . . . . .
H27 H 0.219788 0.565038 0.142699 0.031 Uiso 1 1 calc R U . . .
C13 C 0.7371(5) 0.3436(4) 0.0990(3) 0.0206(10) Uani 1 1 d . . . . .
C16 C 0.9707(5) 0.2913(5) 0.0025(4) 0.0325(13) Uani 1 1 d . . . . .
H16 H 1.050221 0.273034 -0.029517 0.039 Uiso 1 1 calc R U . . .
C24 C 0.3821(5) 0.3505(4) 0.0683(4) 0.0252(11) Uani 1 1 d . . . . .
H24 H 0.349595 0.426719 0.056565 0.030 Uiso 1 1 calc R U . . .
C20 C 0.5381(5) 0.1838(4) 0.1398(4) 0.0241(11) Uani 1 1 d . . . . .
H20 H 0.613681 0.144564 0.176929 0.029 Uiso 1 1 calc R U . . .
C17 C 0.8918(5) 0.2347(5) -0.0039(4) 0.0323(13) Uani 1 1 d . . . . .
H17 H 0.916545 0.178155 -0.041251 0.039 Uiso 1 1 calc R U . . .
C25 C 0.4951(4) 0.5221(4) 0.1502(3) 0.0194(10) Uani 1 1 d . . . . .
H25A H 0.552991 0.561236 0.124250 0.023 Uiso 1 1 calc R U . . .
H25B H 0.427898 0.540199 0.099665 0.023 Uiso 1 1 calc R U . . .
C14 C 0.8192(5) 0.3997(4) 0.1045(4) 0.0240(11) Uani 1 1 d . . . . .
H14 H 0.795807 0.455826 0.142352 0.029 Uiso 1 1 calc R U . . .
C28 C 0.0901(5) 0.5186(5) 0.2318(4) 0.0330(13) Uani 1 1 d . . . . .
H28 H 0.036019 0.523131 0.179102 0.040 Uiso 1 1 calc R U . . .
C18 C 0.7760(5) 0.2602(4) 0.0442(4) 0.0272(11) Uani 1 1 d . . . . .
H18 H 0.722721 0.220352 0.039721 0.033 Uiso 1 1 calc R U . . .
C10 C 0.4320(5) 0.2300(4) 0.3882(4) 0.0256(11) Uani 1 1 d . . . . .
H10 H 0.412080 0.303680 0.347370 0.031 Uiso 1 1 calc R U . . .
C33 C 0.4032(5) 0.7716(4) 0.1661(4) 0.0280(12) Uani 1 1 d . . . . .
H33 H 0.436590 0.740771 0.108818 0.034 Uiso 1 1 calc R U . . .
C11 C 0.4019(5) 0.2413(4) 0.4975(4) 0.0289(12) Uani 1 1 d . . . . .
H11A H 0.429106 0.170035 0.539991 0.043 Uiso 1 1 calc R U . . .
H11B H 0.310972 0.276397 0.504456 0.043 Uiso 1 1 calc R U . . .
H11C H 0.446366 0.284804 0.517884 0.043 Uiso 1 1 calc R U . . .
C6 C 0.5730(5) 0.1712(4) 0.3819(3) 0.0207(10) Uani 1 1 d . . . . .
C30 C 0.1388(5) 0.4832(4) 0.4073(4) 0.0334(13) Uani 1 1 d . . . . .
H30 H 0.116847 0.464513 0.474980 0.040 Uiso 1 1 calc R U . . .
C37 C 0.3384(5) 0.7528(4) 0.3365(4) 0.0297(12) Uani 1 1 d . . . . .
H37 H 0.326283 0.709199 0.396919 0.036 Uiso 1 1 calc R U . . .
C15 C 0.9338(5) 0.3750(5) 0.0557(4) 0.0294(12) Uani 1 1 d . . . . .
H15 H 0.987079 0.415294 0.058785 0.035 Uiso 1 1 calc R U . . .
C12 C 0.3479(5) 0.1769(5) 0.3506(4) 0.0331(13) Uani 1 1 d . . . . .
H12A H 0.365643 0.172193 0.279921 0.050 Uiso 1 1 calc R U . . .
H12B H 0.259263 0.219980 0.357761 0.050 Uiso 1 1 calc R U . . .
H12C H 0.365231 0.104588 0.389935 0.050 Uiso 1 1 calc R U . . .
C5 C 0.6222(6) 0.0608(4) 0.4161(4) 0.0295(12) Uani 1 1 d . . . . .
H5 H 0.565962 0.022492 0.435688 0.035 Uiso 1 1 calc R U . . .
C35 C 0.3236(6) 0.9267(5) 0.2442(4) 0.0350(13) Uani 1 1 d . . . . .
H35 H 0.301418 1.001884 0.240635 0.042 Uiso 1 1 calc R U . . .
C29 C 0.0604(5) 0.4877(4) 0.3301(5) 0.0350(14) Uani 1 1 d . . . . .
H29 H -0.013322 0.469579 0.344903 0.042 Uiso 1 1 calc R U . . .
C4 C 0.7501(6) 0.0055(4) 0.4225(4) 0.0312(13) Uani 1 1 d . . . . .
H4 H 0.781077 -0.070275 0.443586 0.037 Uiso 1 1 calc R U . . .
C36 C 0.3075(6) 0.8627(5) 0.3322(4) 0.0349(13) Uani 1 1 d . . . . .
H36 H 0.275604 0.893652 0.389700 0.042 Uiso 1 1 calc R U . . .
C9 C 1.0012(5) 0.1704(5) 0.2839(4) 0.0338(13) Uani 1 1 d . . . . .
H9A H 1.052407 0.104205 0.327029 0.051 Uiso 1 1 calc R U . . .
H9B H 1.051441 0.216907 0.263281 0.051 Uiso 1 1 calc R U . . .
H9C H 0.973776 0.152791 0.224492 0.051 Uiso 1 1 calc R U . . .
C21 C 0.4740(6) 0.1277(5) 0.1016(4) 0.0323(13) Uani 1 1 d . . . . .
H21 H 0.505532 0.051443 0.113784 0.039 Uiso 1 1 calc R U . . .
C22 C 0.3636(6) 0.1835(5) 0.0456(4) 0.0375(14) Uani 1 1 d . . . . .
H22 H 0.320198 0.145573 0.018930 0.045 Uiso 1 1 calc R U . . .
C8 C 0.9268(6) 0.2446(5) 0.4420(4) 0.0343(13) Uani 1 1 d . . . . .
H8A H 0.853395 0.287772 0.475566 0.051 Uiso 1 1 calc R U . . .
H8B H 0.988436 0.281382 0.429392 0.051 Uiso 1 1 calc R U . . .
H8C H 0.965112 0.174298 0.484690 0.051 Uiso 1 1 calc R U . . .
C42 C 0.9928(7) -0.1228(6) 0.2330(5) 0.0484(17) Uani 1 1 d . . . . .
H42 H 1.068494 -0.110961 0.243956 0.058 Uiso 1 1 calc R U . . .
C41 C 0.9088(8) -0.0525(5) 0.1624(5) 0.055(2) Uani 1 1 d . . . . .
H41 H 0.925210 0.008315 0.125228 0.066 Uiso 1 1 calc R U . . .
C43 C 0.9704(7) -0.2093(6) 0.2879(5) 0.0491(17) Uani 1 1 d . . . . .
H43 H 1.030217 -0.258413 0.336082 0.059 Uiso 1 1 calc R U . . .
C38 C 0.8588(8) -0.2247(6) 0.2723(6) 0.060(2) Uani 1 1 d . . . . .
H38 H 0.841396 -0.284056 0.311358 0.073 Uiso 1 1 calc R U . . .
C39 C 0.7740(8) -0.1563(8) 0.2023(7) 0.071(2) Uani 1 1 d . . . . .
H39 H 0.697440 -0.167198 0.192320 0.085 Uiso 1 1 calc R U . . .
C40 C 0.8006(8) -0.0705(7) 0.1457(6) 0.068(2) Uani 1 1 d . . . . .
H40 H 0.743407 -0.023640 0.094654 0.082 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N1 1.913(4) . ?
Ge1 P3 2.4548(17) . ?
Ge1 Br1 2.5125(10) . ?
P3 C25 1.806(5) . ?
P3 C32 1.815(5) . ?
P3 C26 1.818(5) . ?
Si1 N1 1.729(4) . ?
Si1 C19 1.892(5) . ?
Si1 C13 1.899(5) . ?
Si1 C25 1.912(5) . ?
N1 C1 1.462(6) . ?
C32 C37 1.382(7) . ?
C32 C33 1.394(7) . ?
C7 C2 1.528(7) . ?
C7 C9 1.539(7) . ?
C7 C8 1.542(7) . ?
C19 C20 1.397(7) . ?
C19 C24 1.416(7) . ?
C26 C31 1.385(7) . ?
C26 C27 1.393(7) . ?
C31 C30 1.383(7) . ?
C2 C3 1.388(7) . ?
C2 C1 1.414(7) . ?
C23 C22 1.390(8) . ?
C23 C24 1.397(7) . ?
C1 C6 1.422(6) . ?
C34 C35 1.383(8) . ?
C34 C33 1.384(7) . ?
C3 C4 1.386(7) . ?
C27 C28 1.394(7) . ?
C13 C18 1.397(7) . ?
C13 C14 1.403(7) . ?
C16 C17 1.379(8) . ?
C16 C15 1.386(8) . ?
C20 C21 1.395(7) . ?
C17 C18 1.393(7) . ?
C14 C15 1.386(7) . ?
C28 C29 1.382(8) . ?
C10 C6 1.522(7) . ?
C10 C11 1.530(7) . ?
C10 C12 1.534(7) . ?
C6 C5 1.392(7) . ?
C30 C29 1.395(8) . ?
C37 C36 1.393(8) . ?
C5 C4 1.379(8) . ?
C35 C36 1.381(8) . ?
C21 C22 1.397(9) . ?
C42 C43 1.358(10) . ?
C42 C41 1.364(10) . ?
C41 C40 1.370(11) . ?
C43 C38 1.384(11) . ?
C38 C39 1.357(12) . ?
C39 C40 1.381(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ge1 P3 84.99(12) . . ?
N1 Ge1 Br1 103.02(11) . . ?
P3 Ge1 Br1 84.73(4) . . ?
C25 P3 C32 109.0(2) . . ?
C25 P3 C26 109.7(2) . . ?
C32 P3 C26 106.4(2) . . ?
C25 P3 Ge1 102.39(17) . . ?
C32 P3 Ge1 120.66(16) . . ?
C26 P3 Ge1 108.36(17) . . ?
N1 Si1 C19 114.00(19) . . ?
N1 Si1 C13 113.2(2) . . ?
C19 Si1 C13 105.8(2) . . ?
N1 Si1 C25 103.5(2) . . ?
C19 Si1 C25 111.4(2) . . ?
C13 Si1 C25 109.0(2) . . ?
C1 N1 Si1 119.2(3) . . ?
C1 N1 Ge1 114.3(3) . . ?
Si1 N1 Ge1 126.5(2) . . ?
C37 C32 C33 118.6(5) . . ?
C37 C32 P3 118.4(4) . . ?
C33 C32 P3 123.0(4) . . ?
C2 C7 C9 112.7(4) . . ?
C2 C7 C8 109.8(4) . . ?
C9 C7 C8 109.9(4) . . ?
C20 C19 C24 116.8(4) . . ?
C20 C19 Si1 121.5(4) . . ?
C24 C19 Si1 121.7(4) . . ?
C31 C26 C27 119.8(4) . . ?
C31 C26 P3 117.3(4) . . ?
C27 C26 P3 122.9(4) . . ?
C30 C31 C26 120.2(5) . . ?
C3 C2 C1 118.8(4) . . ?
C3 C2 C7 119.1(4) . . ?
C1 C2 C7 122.0(4) . . ?
C22 C23 C24 120.0(5) . . ?
C2 C1 C6 120.3(4) . . ?
C2 C1 N1 120.6(4) . . ?
C6 C1 N1 119.0(4) . . ?
C35 C34 C33 120.1(5) . . ?
C4 C3 C2 121.2(5) . . ?
C26 C27 C28 120.0(5) . . ?
C18 C13 C14 117.6(4) . . ?
C18 C13 Si1 120.9(4) . . ?
C14 C13 Si1 121.3(4) . . ?
C17 C16 C15 119.9(5) . . ?
C23 C24 C19 121.7(5) . . ?
C21 C20 C19 122.0(5) . . ?
C16 C17 C18 120.2(5) . . ?
P3 C25 Si1 109.6(2) . . ?
C15 C14 C13 121.3(5) . . ?
C29 C28 C27 120.0(5) . . ?
C17 C18 C13 121.0(5) . . ?
C6 C10 C11 107.5(4) . . ?
C6 C10 C12 115.3(4) . . ?
C11 C10 C12 110.0(4) . . ?
C34 C33 C32 120.7(5) . . ?
C5 C6 C1 117.8(5) . . ?
C5 C6 C10 119.5(4) . . ?
C1 C6 C10 122.5(4) . . ?
C31 C30 C29 120.2(5) . . ?
C32 C37 C36 120.9(5) . . ?
C14 C15 C16 119.9(5) . . ?
C4 C5 C6 121.9(5) . . ?
C36 C35 C34 119.9(5) . . ?
C28 C29 C30 119.8(5) . . ?
C5 C4 C3 119.6(5) . . ?
C35 C36 C37 119.8(5) . . ?
C20 C21 C22 120.1(5) . . ?
C23 C22 C21 119.4(5) . . ?
C43 C42 C41 121.4(7) . . ?
C42 C41 C40 119.2(7) . . ?
C42 C43 C38 118.8(7) . . ?
C39 C38 C43 121.1(8) . . ?
C38 C39 C40 118.9(8) . . ?
C41 C40 C39 120.6(8) . . ?

_refine_diff_density_max         0.793
_refine_diff_density_min         -1.117
_refine_diff_density_rms         0.150


####################################################################### 
# 
# 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_compound_PhiPDippNH
_database_code_depnum_ccdc_archive 'CCDC 2057308'
loop_
_audit_author_name
_audit_author_address
'Terrance Hadlington'
;TU Munich
Germany
;
_audit_update_record             
;
2021-01-19 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H44 N P Si'
_chemical_formula_sum            'C31 H44 N P Si'
_chemical_formula_weight         489.73

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   35.733(7)
_cell_length_b                   9.7400(19)
_cell_length_c                   17.970(4)
_cell_angle_alpha                90
_cell_angle_beta                 107.22(3)
_cell_angle_gamma                90
_cell_volume                     5974(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2000
_cell_measurement_theta_min      1.92
_cell_measurement_theta_max      32.50

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.27
_exptl_absorpt_coefficient_mu    0.150
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.953
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'STOE X-AREA 1.76'

_diffrn_ambient_temperature      150(2)
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            21921
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.956
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5840
_reflns_number_gt                4192
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0809P)²+2.4655P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5840
_refine_ls_number_parameters     316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0489
_refine_ls_wR_factor_ref         0.1441
_refine_ls_wR_factor_gt          0.1283
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_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
P1 P 0.12423(2) 0.36190(6) 0.32839(3) 0.03023(17) Uani 1 1 d . . . . .
Si1 Si 0.11178(2) 0.24693(6) 0.48429(3) 0.02308(16) Uani 1 1 d . . . . .
N1 N 0.11363(5) 0.09176(18) 0.43609(10) 0.0274(4) Uani 1 1 d . . . . .
C1 C 0.13235(6) -0.0325(2) 0.46958(12) 0.0251(4) Uani 1 1 d . . . . .
C19 C 0.13623(6) 0.3785(2) 0.43649(12) 0.0273(5) Uani 1 1 d . . . . .
H19A H 0.128462 0.471346 0.448828 0.033 Uiso 1 1 calc R U . . .
H19B H 0.164973 0.370695 0.459536 0.033 Uiso 1 1 calc R U . . .
C26 C 0.17015(7) 0.4210(2) 0.31172(12) 0.0301(5) Uani 1 1 d . . . . .
C25 C 0.09804(7) 0.6431(2) 0.32248(14) 0.0341(5) Uani 1 1 d . . . . .
H25 H 0.119388 0.659613 0.367771 0.041 Uiso 1 1 calc R U . . .
C6 C 0.16749(6) -0.0751(2) 0.45523(13) 0.0282(5) Uani 1 1 d . . . . .
C2 C 0.11565(6) -0.1135(2) 0.51753(13) 0.0288(5) Uani 1 1 d . . . . .
C3 C 0.13455(7) -0.2346(2) 0.54952(14) 0.0353(5) Uani 1 1 d . . . . .
H3 H 0.123592 -0.289221 0.581602 0.042 Uiso 1 1 calc R U . . .
C13 C 0.14095(7) 0.2286(2) 0.59044(13) 0.0296(5) Uani 1 1 d . . . . .
H13 H 0.131959 0.142087 0.609752 0.036 Uiso 1 1 calc R U . . .
C5 C 0.18511(7) -0.1971(2) 0.48886(14) 0.0341(5) Uani 1 1 d . . . . .
H5 H 0.208701 -0.226353 0.479609 0.041 Uiso 1 1 calc R U . . .
C20 C 0.09164(6) 0.5103(2) 0.29122(13) 0.0306(5) Uani 1 1 d . . . . .
C7 C 0.07667(7) -0.0746(2) 0.53062(14) 0.0321(5) Uani 1 1 d . . . . .
H7 H 0.072739 0.025893 0.519807 0.038 Uiso 1 1 calc R U . . .
C31 C 0.19307(7) 0.5272(2) 0.35362(14) 0.0363(5) Uani 1 1 d . . . . .
H31 H 0.185278 0.571689 0.393688 0.044 Uiso 1 1 calc R U . . .
C10 C 0.18547(7) 0.0103(2) 0.40281(14) 0.0340(5) Uani 1 1 d . . . . .
H10 H 0.177357 0.107895 0.405996 0.041 Uiso 1 1 calc R U . . .
C16 C 0.05927(7) 0.2993(2) 0.47267(14) 0.0340(5) Uani 1 1 d . . . . .
H16 H 0.051062 0.253031 0.515001 0.041 Uiso 1 1 calc R U . . .
C27 C 0.18285(8) 0.3558(3) 0.25376(14) 0.0385(6) Uani 1 1 d . . . . .
H27 H 0.168082 0.281738 0.225108 0.046 Uiso 1 1 calc R U . . .
C29 C 0.23887(7) 0.5056(3) 0.27915(15) 0.0460(7) Uani 1 1 d . . . . .
H29 H 0.261810 0.535334 0.267437 0.055 Uiso 1 1 calc R U . . .
C30 C 0.22719(7) 0.5693(3) 0.33786(15) 0.0419(6) Uani 1 1 d . . . . .
H30 H 0.242499 0.641541 0.367242 0.050 Uiso 1 1 calc R U . . .
C4 C 0.16884(7) -0.2770(2) 0.53569(14) 0.0372(6) Uani 1 1 d . . . . .
H4 H 0.181192 -0.359934 0.557942 0.045 Uiso 1 1 calc R U . . .
C14 C 0.13390(8) 0.3458(3) 0.64177(15) 0.0472(7) Uani 1 1 d . . . . .
H14A H 0.149689 0.330422 0.695839 0.071 Uiso 1 1 calc R U . . .
H14B H 0.106094 0.348595 0.638913 0.071 Uiso 1 1 calc R U . . .
H14C H 0.141415 0.433291 0.623329 0.071 Uiso 1 1 calc R U . . .
C28 C 0.21682(8) 0.3985(3) 0.23799(16) 0.0483(7) Uani 1 1 d . . . . .
H28 H 0.224971 0.353691 0.198463 0.058 Uiso 1 1 calc R U . . .
C21 C 0.05973(7) 0.4887(3) 0.22554(14) 0.0396(6) Uani 1 1 d . . . . .
H21 H 0.054596 0.399067 0.204055 0.048 Uiso 1 1 calc R U . . .
C8 C 0.04262(7) -0.1493(3) 0.47252(18) 0.0502(7) Uani 1 1 d . . . . .
H8A H 0.043315 -0.130865 0.419335 0.075 Uiso 1 1 calc R U . . .
H8B H 0.017745 -0.116442 0.478521 0.075 Uiso 1 1 calc R U . . .
H8C H 0.045002 -0.248278 0.482542 0.075 Uiso 1 1 calc R U . . .
C24 C 0.07343(7) 0.7514(3) 0.28786(15) 0.0405(6) Uani 1 1 d . . . . .
H24 H 0.078004 0.840853 0.309777 0.049 Uiso 1 1 calc R U . . .
C18 C 0.05497(8) 0.4548(3) 0.48211(18) 0.0472(7) Uani 1 1 d . . . . .
H18A H 0.061992 0.503265 0.440336 0.071 Uiso 1 1 calc R U . . .
H18B H 0.072390 0.484214 0.532678 0.071 Uiso 1 1 calc R U . . .
H18C H 0.027787 0.476159 0.479317 0.071 Uiso 1 1 calc R U . . .
C12 C 0.16917(8) -0.0348(3) 0.31753(14) 0.0434(6) Uani 1 1 d . . . . .
H12A H 0.177465 -0.129232 0.312015 0.065 Uiso 1 1 calc R U . . .
H12B H 0.179151 0.026276 0.284435 0.065 Uiso 1 1 calc R U . . .
H12C H 0.140494 -0.030388 0.301640 0.065 Uiso 1 1 calc R U . . .
C23 C 0.04244(7) 0.7286(3) 0.22181(16) 0.0468(7) Uani 1 1 d . . . . .
H23 H 0.026060 0.802669 0.197440 0.056 Uiso 1 1 calc R U . . .
C22 C 0.03530(8) 0.5967(3) 0.19106(16) 0.0508(7) Uani 1 1 d . . . . .
H22 H 0.013630 0.580454 0.146317 0.061 Uiso 1 1 calc R U . . .
C17 C 0.03124(7) 0.2508(3) 0.39438(17) 0.0475(7) Uani 1 1 d . . . . .
H17A H 0.004269 0.274842 0.391893 0.071 Uiso 1 1 calc R U . . .
H17B H 0.033401 0.151027 0.389915 0.071 Uiso 1 1 calc R U . . .
H17C H 0.038225 0.295666 0.351510 0.071 Uiso 1 1 calc R U . . .
C15 C 0.18483(7) 0.2129(3) 0.60183(16) 0.0491(7) Uani 1 1 d . . . . .
H15A H 0.195138 0.298263 0.586660 0.074 Uiso 1 1 calc R U . . .
H15B H 0.189194 0.137270 0.569411 0.074 Uiso 1 1 calc R U . . .
H15C H 0.198297 0.193164 0.656709 0.074 Uiso 1 1 calc R U . . .
C9 C 0.07567(9) -0.0983(3) 0.61473(17) 0.0576(8) Uani 1 1 d . . . . .
H9A H 0.076822 -0.197039 0.625736 0.086 Uiso 1 1 calc R U . . .
H9B H 0.051362 -0.060344 0.620898 0.086 Uiso 1 1 calc R U . . .
H9C H 0.098178 -0.052677 0.651080 0.086 Uiso 1 1 calc R U . . .
C11 C 0.23033(8) 0.0071(3) 0.42759(18) 0.0574(8) Uani 1 1 d . . . . .
H11A H 0.240546 0.033177 0.482574 0.086 Uiso 1 1 calc R U . . .
H11B H 0.239910 0.071812 0.395650 0.086 Uiso 1 1 calc R U . . .
H11C H 0.239233 -0.085777 0.420420 0.086 Uiso 1 1 calc R U . . .
H1 H 0.117349 0.103626 0.387115 0.063(9) Uiso 1 1 d R . . . .


_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
P1 C26 1.845(2) . ?
P1 C20 1.852(2) . ?
P1 C19 1.868(2) . ?
Si1 N1 1.7528(18) . ?
Si1 C13 1.892(2) . ?
Si1 C19 1.894(2) . ?
Si1 C16 1.895(2) . ?
N1 C1 1.427(3) . ?
C1 C6 1.417(3) . ?
C1 C2 1.423(3) . ?
C26 C31 1.394(3) . ?
C26 C27 1.405(3) . ?
C25 C24 1.396(3) . ?
C25 C20 1.402(3) . ?
C6 C5 1.396(3) . ?
C6 C10 1.533(3) . ?
C2 C3 1.395(3) . ?
C2 C7 1.527(3) . ?
C3 C4 1.384(3) . ?
C13 C15 1.528(3) . ?
C13 C14 1.535(3) . ?
C5 C4 1.393(3) . ?
C20 C21 1.393(3) . ?
C7 C8 1.532(3) . ?
C7 C9 1.540(3) . ?
C31 C30 1.392(3) . ?
C10 C11 1.532(3) . ?
C10 C12 1.534(3) . ?
C16 C18 1.537(3) . ?
C16 C17 1.540(4) . ?
C27 C28 1.389(4) . ?
C29 C28 1.382(4) . ?
C29 C30 1.390(4) . ?
C21 C22 1.391(4) . ?
C24 C23 1.381(4) . ?
C23 C22 1.392(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C26 P1 C20 101.09(10) . . ?
C26 P1 C19 101.55(10) . . ?
C20 P1 C19 103.52(10) . . ?
N1 Si1 C13 109.08(9) . . ?
N1 Si1 C19 105.63(9) . . ?
C13 Si1 C19 109.30(10) . . ?
N1 Si1 C16 111.00(10) . . ?
C13 Si1 C16 111.62(11) . . ?
C19 Si1 C16 110.02(10) . . ?
C1 N1 Si1 127.20(15) . . ?
C6 C1 C2 120.09(19) . . ?
C6 C1 N1 120.10(18) . . ?
C2 C1 N1 119.81(19) . . ?
P1 C19 Si1 114.72(11) . . ?
C31 C26 C27 118.0(2) . . ?
C31 C26 P1 123.55(17) . . ?
C27 C26 P1 118.48(19) . . ?
C24 C25 C20 120.8(2) . . ?
C5 C6 C1 118.7(2) . . ?
C5 C6 C10 120.7(2) . . ?
C1 C6 C10 120.56(19) . . ?
C3 C2 C1 118.6(2) . . ?
C3 C2 C7 119.88(19) . . ?
C1 C2 C7 121.40(19) . . ?
C4 C3 C2 121.7(2) . . ?
C15 C13 C14 109.8(2) . . ?
C15 C13 Si1 112.44(16) . . ?
C14 C13 Si1 113.35(17) . . ?
C4 C5 C6 121.5(2) . . ?
C21 C20 C25 118.3(2) . . ?
C21 C20 P1 117.22(18) . . ?
C25 C20 P1 124.40(18) . . ?
C2 C7 C8 110.73(19) . . ?
C2 C7 C9 113.7(2) . . ?
C8 C7 C9 110.7(2) . . ?
C30 C31 C26 121.2(2) . . ?
C11 C10 C6 113.8(2) . . ?
C11 C10 C12 109.9(2) . . ?
C6 C10 C12 110.74(19) . . ?
C18 C16 C17 110.1(2) . . ?
C18 C16 Si1 112.41(16) . . ?
C17 C16 Si1 111.90(17) . . ?
C28 C27 C26 120.6(2) . . ?
C28 C29 C30 119.4(2) . . ?
C29 C30 C31 120.0(3) . . ?
C3 C4 C5 119.4(2) . . ?
C29 C28 C27 120.7(2) . . ?
C22 C21 C20 120.8(2) . . ?
C23 C24 C25 120.0(2) . . ?
C24 C23 C22 119.7(3) . . ?
C21 C22 C23 120.3(2) . . ?

_refine_diff_density_max         1.317
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.054


####################################################################### 
# 
# 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_compound_2
_database_code_depnum_ccdc_archive 'CCDC 2057298'
loop_
_audit_author_name
_audit_author_address
'Terrance Hadlington'
;TU Munich
Germany
;
_audit_update_record             
;
2021-01-19 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT602_compound_2          
;
PROBLEM: Solvent Accessible VOID(S) in Structure ........          ! Check
RESPONSE: The SQUEEZE funation was used to removed electron density relating to highly disordered solvent molecules. See CIF for details.
;
# Added during the CSD deposition process: Tuesday 19 January 2021 04:01 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C74 H78 Br6 Ge2 N2 Ni2 P2 Si2'
_chemical_formula_sum            'C74 H78 Br6 Ge2 N2 Ni2 P2 Si2'
_chemical_formula_weight         1855.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'
Ni Ni 0.3393 1.1124 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   40.613(8)
_cell_length_b                   9.870(2)
_cell_length_c                   23.160(5)
_cell_angle_alpha                90
_cell_angle_beta                 101.59(3)
_cell_angle_gamma                90
_cell_volume                     9094(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2000
_cell_measurement_theta_min      1.92
_cell_measurement_theta_max      32.5

_exptl_crystal_description       rod
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_F_000             3696
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    3.795
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'STOE X-AREA 1.76'

_diffrn_ambient_temperature      150(2)
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            8903
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_av_R_equivalents  0.0897
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_theta_min         2.716
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             8903
_reflns_number_gt                6105
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.250  0.250  0.000       645       113 'C28 H32'
   2  0.250 -0.250  0.500       645       113 'C28 H32'
   3  0.750 -0.250  0.000       645       113 'C28 H32'
   4  0.750  0.250  0.500       645       113 'C28 H32'
   5  0.000  0.177  0.750         8         0 ' '
   6  0.500  0.323  0.250         8         0 ' '
   7  0.500  0.677  0.750         8         0 ' '
   8  0.000  0.823  0.250         8         0 ' ',SQUEEZE
;
_platon_squeeze_details          
;
The unit cell contains 16 toluene molecules (4 per asymmetric unit) which have been treated
as a diffuse contribution to the overall scattering without specific atom
positions by SQUEEZE/PLATON.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0939P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8903
_refine_ls_number_parameters     410
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0470
_refine_ls_wR_factor_ref         0.1402
_refine_ls_wR_factor_gt          0.1270
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_restrained_S_all      0.970
_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
Ge1 Ge 0.58954(2) 0.68830(5) 0.30205(2) 0.02560(14) Uani 1 1 d . . . . .
Br3 Br 0.51383(2) 0.59783(6) 0.32094(3) 0.04359(16) Uani 1 1 d . . . . .
Br2 Br 0.59672(2) 0.92119(5) 0.32427(3) 0.04368(16) Uani 1 1 d . . . . .
Br1 Br 0.59656(2) 0.60222(6) 0.39753(3) 0.04530(17) Uani 1 1 d . . . . .
Ni1 Ni 0.53867(2) 0.65245(6) 0.24114(3) 0.02715(16) Uani 1 1 d . . . . .
P1 P 0.55819(3) 0.72918(13) 0.16697(6) 0.0281(3) Uani 1 1 d . . . . .
Si1 Si 0.63905(3) 0.68659(13) 0.21350(6) 0.0260(3) Uani 1 1 d . . . . .
N1 N 0.62871(9) 0.6317(4) 0.27939(17) 0.0248(8) Uani 1 1 d . . . . .
C1 C 0.64674(11) 0.5194(5) 0.3106(2) 0.0271(10) Uani 1 1 d . . . . .
C13 C 0.67527(11) 0.8104(4) 0.2231(2) 0.0295(11) Uani 1 1 d . . . . .
C2 C 0.67574(12) 0.5447(5) 0.3549(2) 0.0338(11) Uani 1 1 d . . . . .
C26 C 0.55263(12) 0.6145(5) 0.1036(2) 0.0333(11) Uani 1 1 d . . . . .
C25 C 0.60151(11) 0.7891(5) 0.1751(2) 0.0278(10) Uani 1 1 d . . . . .
H25A H 0.602686 0.877289 0.195841 0.033 Uiso 1 1 calc R U . . .
H25B H 0.605122 0.808402 0.134916 0.033 Uiso 1 1 calc R U . . .
C6 C 0.63525(12) 0.3862(5) 0.2971(2) 0.0338(12) Uani 1 1 d . . . . .
C32 C 0.53211(12) 0.8795(5) 0.1434(2) 0.0348(12) Uani 1 1 d . . . . .
C19 C 0.65223(12) 0.5435(5) 0.1702(2) 0.0314(11) Uani 1 1 d . . . . .
C20 C 0.67953(12) 0.4624(5) 0.1944(2) 0.0365(12) Uani 1 1 d . . . . .
H20 H 0.689844 0.475132 0.234635 0.044 Uiso 1 1 calc R U . . .
C18 C 0.70298(12) 0.7874(5) 0.1968(2) 0.0339(11) Uani 1 1 d . . . . .
H18 H 0.704024 0.706859 0.174763 0.041 Uiso 1 1 calc R U . . .
C10 C 0.60370(13) 0.3523(5) 0.2528(3) 0.0372(12) Uani 1 1 d . . . . .
H10 H 0.595945 0.436852 0.230399 0.045 Uiso 1 1 calc R U . . .
C7 C 0.68775(13) 0.6872(6) 0.3737(2) 0.0383(12) Uani 1 1 d . . . . .
H7 H 0.671990 0.753054 0.349591 0.046 Uiso 1 1 calc R U . . .
C5 C 0.65431(15) 0.2794(5) 0.3280(3) 0.0442(14) Uani 1 1 d . . . . .
H5 H 0.647062 0.188488 0.320152 0.053 Uiso 1 1 calc R U . . .
C21 C 0.69232(14) 0.3643(6) 0.1626(3) 0.0421(13) Uani 1 1 d . . . . .
H21 H 0.710980 0.310715 0.180727 0.051 Uiso 1 1 calc R U . . .
C16 C 0.72800(13) 0.9998(6) 0.2342(3) 0.0468(14) Uani 1 1 d . . . . .
H16 H 0.745877 1.063385 0.238253 0.056 Uiso 1 1 calc R U . . .
C14 C 0.67492(13) 0.9297(5) 0.2544(3) 0.0388(12) Uani 1 1 d . . . . .
H14 H 0.656508 0.947573 0.272916 0.047 Uiso 1 1 calc R U . . .
C27 C 0.54552(13) 0.4780(6) 0.1094(3) 0.0408(13) Uani 1 1 d . . . . .
H27 H 0.542858 0.444350 0.146645 0.049 Uiso 1 1 calc R U . . .
C17 C 0.72904(13) 0.8815(6) 0.2026(3) 0.0438(14) Uani 1 1 d . . . . .
H17 H 0.747704 0.864218 0.184705 0.053 Uiso 1 1 calc R U . . .
C3 C 0.69381(14) 0.4354(6) 0.3825(3) 0.0464(14) Uani 1 1 d . . . . .
H3 H 0.713827 0.450544 0.410971 0.056 Uiso 1 1 calc R U . . .
C31 C 0.55668(14) 0.6610(6) 0.0487(2) 0.0430(13) Uani 1 1 d . . . . .
H31 H 0.562365 0.753191 0.044005 0.052 Uiso 1 1 calc R U . . .
C24 C 0.63815(13) 0.5220(6) 0.1102(2) 0.0411(13) Uani 1 1 d . . . . .
H24 H 0.619549 0.575436 0.091721 0.049 Uiso 1 1 calc R U . . .
C15 C 0.70085(14) 1.0241(5) 0.2596(3) 0.0465(14) Uani 1 1 d . . . . .
H15 H 0.699710 1.105824 0.280773 0.056 Uiso 1 1 calc R U . . .
C4 C 0.68285(15) 0.3041(6) 0.3689(3) 0.0512(16) Uani 1 1 d . . . . .
H4 H 0.695425 0.230243 0.388274 0.061 Uiso 1 1 calc R U . . .
C30 C 0.55244(15) 0.5728(7) 0.0004(3) 0.0533(16) Uani 1 1 d . . . . .
H30 H 0.554713 0.605362 -0.037173 0.064 Uiso 1 1 calc R U . . .
C9 C 0.68700(16) 0.7116(7) 0.4388(3) 0.0549(16) Uani 1 1 d . . . . .
H9A H 0.664384 0.692987 0.445604 0.082 Uiso 1 1 calc R U . . .
H9B H 0.692956 0.806029 0.448967 0.082 Uiso 1 1 calc R U . . .
H9C H 0.703182 0.651291 0.463408 0.082 Uiso 1 1 calc R U . . .
C11 C 0.57565(15) 0.3082(6) 0.2859(3) 0.0562(17) Uani 1 1 d . . . . .
H11A H 0.581950 0.222201 0.306267 0.084 Uiso 1 1 calc R U . . .
H11B H 0.554441 0.296764 0.257436 0.084 Uiso 1 1 calc R U . . .
H11C H 0.572910 0.377830 0.314684 0.084 Uiso 1 1 calc R U . . .
C29 C 0.54507(15) 0.4404(7) 0.0076(3) 0.0551(16) Uani 1 1 d . . . . .
H29 H 0.541784 0.380847 -0.025279 0.066 Uiso 1 1 calc R U . . .
C22 C 0.67739(16) 0.3450(6) 0.1033(3) 0.0537(16) Uani 1 1 d . . . . .
H22 H 0.685628 0.276942 0.080919 0.064 Uiso 1 1 calc R U . . .
C12 C 0.60885(15) 0.2437(6) 0.2080(3) 0.0514(15) Uani 1 1 d . . . . .
H12A H 0.626660 0.272611 0.187793 0.077 Uiso 1 1 calc R U . . .
H12B H 0.587882 0.231104 0.179068 0.077 Uiso 1 1 calc R U . . .
H12C H 0.615282 0.157986 0.228576 0.077 Uiso 1 1 calc R U . . .
C8 C 0.72304(14) 0.7143(7) 0.3626(3) 0.0509(15) Uani 1 1 d . . . . .
H8A H 0.738973 0.650992 0.385964 0.076 Uiso 1 1 calc R U . . .
H8B H 0.729657 0.807469 0.374219 0.076 Uiso 1 1 calc R U . . .
H8C H 0.723122 0.701888 0.320690 0.076 Uiso 1 1 calc R U . . .
C23 C 0.65090(16) 0.4245(6) 0.0778(3) 0.0539(16) Uani 1 1 d . . . . .
H23 H 0.641121 0.412755 0.037227 0.065 Uiso 1 1 calc R U . . .
C28 C 0.54230(15) 0.3915(6) 0.0625(3) 0.0526(16) Uani 1 1 d . . . . .
H28 H 0.538158 0.297953 0.067591 0.063 Uiso 1 1 calc R U . . .
C37 C 0.53327(17) 0.9862(6) 0.1810(3) 0.0628(19) Uani 1 1 d . . . . .
H37 H 0.549168 0.984286 0.217201 0.075 Uiso 1 1 calc R U . . .
C33 C 0.50863(19) 0.8844(8) 0.0893(3) 0.073(2) Uani 1 1 d . . . . .
H33 H 0.507062 0.810678 0.062461 0.088 Uiso 1 1 calc R U . . .
C36 C 0.51236(19) 1.0965(7) 0.1687(4) 0.079(2) Uani 1 1 d . . . . .
H36 H 0.513031 1.166860 0.196923 0.094 Uiso 1 1 calc R U . . .
C35 C 0.49056(18) 1.1038(8) 0.1154(4) 0.073(2) Uani 1 1 d . . . . .
H35 H 0.477038 1.182171 0.105240 0.087 Uiso 1 1 calc R U . . .
C34 C 0.48827(19) 0.9941(10) 0.0754(3) 0.086(3) Uani 1 1 d . . . . .
H34 H 0.472572 0.997093 0.038970 0.104 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N1 1.859(4) . ?
Ge1 Ni1 2.2828(10) . ?
Ge1 Br1 2.3324(9) . ?
Ge1 Br2 2.3608(8) . ?
Br3 Ni1 2.3395(10) . ?
Br3 Ni1 2.3820(11) 2_655 ?
Ni1 P1 2.1679(14) . ?
P1 C25 1.830(5) . ?
P1 C26 1.832(5) . ?
P1 C32 1.841(5) . ?
Si1 N1 1.748(4) . ?
Si1 C19 1.871(5) . ?
Si1 C13 1.891(5) . ?
Si1 C25 1.896(5) . ?
N1 C1 1.440(6) . ?
C1 C6 1.408(7) . ?
C1 C2 1.421(7) . ?
C13 C14 1.384(7) . ?
C13 C18 1.401(7) . ?
C2 C3 1.387(7) . ?
C2 C7 1.522(7) . ?
C26 C27 1.390(7) . ?
C26 C31 1.391(8) . ?
C6 C5 1.415(7) . ?
C6 C10 1.508(8) . ?
C32 C37 1.362(8) . ?
C32 C33 1.415(9) . ?
C19 C20 1.391(7) . ?
C19 C24 1.408(7) . ?
C20 C21 1.379(7) . ?
C18 C17 1.394(7) . ?
C10 C12 1.535(8) . ?
C10 C11 1.557(8) . ?
C7 C8 1.529(7) . ?
C7 C9 1.534(8) . ?
C5 C4 1.363(9) . ?
C21 C22 1.398(9) . ?
C16 C15 1.371(8) . ?
C16 C17 1.383(8) . ?
C14 C15 1.394(7) . ?
C27 C28 1.367(8) . ?
C3 C4 1.385(9) . ?
C31 C30 1.401(8) . ?
C24 C23 1.384(8) . ?
C30 C29 1.358(9) . ?
C29 C28 1.386(9) . ?
C22 C23 1.367(9) . ?
C37 C36 1.375(9) . ?
C33 C34 1.362(10) . ?
C36 C35 1.370(11) . ?
C35 C34 1.415(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ge1 Ni1 119.91(12) . . ?
N1 Ge1 Br1 102.10(12) . . ?
Ni1 Ge1 Br1 116.91(4) . . ?
N1 Ge1 Br2 106.19(12) . . ?
Ni1 Ge1 Br2 110.03(3) . . ?
Br1 Ge1 Br2 99.31(3) . . ?
Ni1 Br3 Ni1 86.96(3) . 2_655 ?
P1 Ni1 Ge1 90.35(4) . . ?
P1 Ni1 Br3 172.22(5) . . ?
Ge1 Ni1 Br3 91.60(3) . . ?
P1 Ni1 Br3 91.51(5) . 2_655 ?
Ge1 Ni1 Br3 175.82(3) . 2_655 ?
Br3 Ni1 Br3 87.06(4) . 2_655 ?
C25 P1 C26 104.1(2) . . ?
C25 P1 C32 104.7(2) . . ?
C26 P1 C32 106.8(2) . . ?
C25 P1 Ni1 121.88(16) . . ?
C26 P1 Ni1 114.44(17) . . ?
C32 P1 Ni1 103.70(17) . . ?
N1 Si1 C19 112.2(2) . . ?
N1 Si1 C13 114.6(2) . . ?
C19 Si1 C13 104.6(2) . . ?
N1 Si1 C25 105.24(19) . . ?
C19 Si1 C25 116.2(2) . . ?
C13 Si1 C25 104.1(2) . . ?
C1 N1 Si1 119.3(3) . . ?
C1 N1 Ge1 117.9(3) . . ?
Si1 N1 Ge1 121.5(2) . . ?
C6 C1 C2 121.0(4) . . ?
C6 C1 N1 119.6(4) . . ?
C2 C1 N1 119.4(4) . . ?
C14 C13 C18 117.4(4) . . ?
C14 C13 Si1 121.4(4) . . ?
C18 C13 Si1 121.2(4) . . ?
C3 C2 C1 118.8(5) . . ?
C3 C2 C7 118.5(5) . . ?
C1 C2 C7 122.7(4) . . ?
C27 C26 C31 118.3(5) . . ?
C27 C26 P1 121.0(4) . . ?
C31 C26 P1 120.7(4) . . ?
P1 C25 Si1 122.8(2) . . ?
C1 C6 C5 117.4(5) . . ?
C1 C6 C10 123.8(4) . . ?
C5 C6 C10 118.8(5) . . ?
C37 C32 C33 118.1(5) . . ?
C37 C32 P1 119.3(4) . . ?
C33 C32 P1 122.4(5) . . ?
C20 C19 C24 116.3(5) . . ?
C20 C19 Si1 120.6(4) . . ?
C24 C19 Si1 122.6(4) . . ?
C21 C20 C19 123.0(5) . . ?
C17 C18 C13 120.7(5) . . ?
C6 C10 C12 113.7(4) . . ?
C6 C10 C11 109.5(5) . . ?
C12 C10 C11 110.5(4) . . ?
C2 C7 C8 111.8(5) . . ?
C2 C7 C9 110.9(5) . . ?
C8 C7 C9 109.9(5) . . ?
C4 C5 C6 121.3(5) . . ?
C20 C21 C22 119.0(5) . . ?
C15 C16 C17 119.2(5) . . ?
C13 C14 C15 121.7(5) . . ?
C28 C27 C26 121.1(5) . . ?
C16 C17 C18 120.7(5) . . ?
C4 C3 C2 120.4(5) . . ?
C26 C31 C30 120.4(6) . . ?
C23 C24 C19 121.2(5) . . ?
C16 C15 C14 120.3(5) . . ?
C5 C4 C3 121.0(5) . . ?
C29 C30 C31 119.7(6) . . ?
C30 C29 C28 120.5(6) . . ?
C23 C22 C21 119.7(5) . . ?
C22 C23 C24 120.8(6) . . ?
C27 C28 C29 119.9(6) . . ?
C32 C37 C36 122.6(6) . . ?
C34 C33 C32 120.4(7) . . ?
C35 C36 C37 119.3(7) . . ?
C36 C35 C34 119.7(6) . . ?
C33 C34 C35 119.8(7) . . ?

_refine_diff_density_max         0.662
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.121


####################################################################### 
# 
# 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_compound_PhPhDippNK
_database_code_depnum_ccdc_archive 'CCDC 2057309'
loop_
_audit_author_name
_audit_author_address
'Terrance Hadlington'
;TU Munich
Germany
;
_audit_update_record             
;
2021-01-19 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H63 K N2 O2 P Si'
_chemical_formula_sum            'C48 H63 K N2 O2 P Si'
_chemical_formula_weight         798.16

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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                   11.280(2)
_cell_length_b                   13.730(3)
_cell_length_c                   15.610(3)
_cell_angle_alpha                84.30(3)
_cell_angle_beta                 83.70(3)
_cell_angle_gamma                72.90(3)
_cell_volume                     2291.0(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2000
_cell_measurement_theta_min      1.92
_cell_measurement_theta_max      32.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_F_000             858
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    0.215
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.964
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'STOE X-AREA 1.76'

_diffrn_ambient_temperature      150(2)
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            22863
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.962
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8979
_reflns_number_gt                6582
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1145P)²+1.4189P] 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         8979
_refine_ls_number_parameters     543
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0641
_refine_ls_wR_factor_ref         0.1979
_refine_ls_wR_factor_gt          0.1764
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.008
_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
K001 K 0.10721(6) 0.35797(5) 0.72546(4) 0.04667(19) Uani 1 1 d . . . . .
Si1 Si 0.40363(6) 0.14290(5) 0.76175(4) 0.03211(19) Uani 1 1 d . . . . .
P1 P 0.27036(8) 0.15997(6) 0.59403(5) 0.0448(2) Uani 1 1 d . . . . .
N1 N 0.3379(2) 0.26340(16) 0.78317(13) 0.0338(5) Uani 1 1 d . . . . .
O2 O -0.1086(6) 0.3402(5) 0.8112(5) 0.0553(13) Uani 0.716(12) 1 d . . P A 1
C1 C 0.3758(2) 0.33968(19) 0.81221(15) 0.0316(5) Uani 1 1 d . . . . .
C6 C 0.3744(2) 0.3518(2) 0.90283(16) 0.0353(6) Uani 1 1 d . . . . .
O1 O 0.0378(6) 0.5496(4) 0.7799(7) 0.077(2) Uani 0.716(12) 1 d . . P A 1
C25 C 0.4220(3) 0.1233(2) 0.64082(18) 0.0425(6) Uani 1 1 d . . . . .
H25A H 0.474474 0.164693 0.610493 0.051 Uiso 1 1 calc R U . . .
H25B H 0.465008 0.050590 0.631769 0.051 Uiso 1 1 calc R U . . .
C13 C 0.5648(2) 0.0810(2) 0.80074(19) 0.0404(6) Uani 1 1 d . . . . .
C19 C 0.3036(2) 0.0592(2) 0.81170(17) 0.0359(6) Uani 1 1 d . . . . .
C5 C 0.4052(3) 0.4340(2) 0.92996(18) 0.0438(7) Uani 1 1 d . . . . .
H5 H 0.403302 0.440580 0.990139 0.053 Uiso 1 1 calc R U . . .
C14 C 0.5775(3) 0.0419(2) 0.8867(2) 0.0500(7) Uani 1 1 d . . . . .
H14 H 0.504424 0.046278 0.924564 0.060 Uiso 1 1 calc R U . . .
C24 C 0.1865(3) 0.0986(2) 0.85651(18) 0.0400(6) Uani 1 1 d . . . . .
H24 H 0.155717 0.170108 0.862377 0.048 Uiso 1 1 calc R U . . .
C2 C 0.4105(3) 0.4158(2) 0.75324(16) 0.0391(6) Uani 1 1 d . . . . .
C23 C 0.1142(3) 0.0353(3) 0.8926(2) 0.0492(7) Uani 1 1 d . . . . .
H23 H 0.035112 0.064097 0.922117 0.059 Uiso 1 1 calc R U . . .
C10 C 0.3325(3) 0.2771(2) 0.96849(17) 0.0440(7) Uani 1 1 d . . . . .
H10 H 0.349554 0.211505 0.940313 0.053 Uiso 1 1 calc R U . . .
C4 C 0.4388(3) 0.5069(3) 0.87183(19) 0.0512(8) Uani 1 1 d . . . . .
H4 H 0.459109 0.562696 0.891758 0.061 Uiso 1 1 calc R U . . .
C3 C 0.4419(3) 0.4962(3) 0.78416(19) 0.0503(8) Uani 1 1 d . . . . .
H3 H 0.466157 0.544938 0.743968 0.060 Uiso 1 1 calc R U . . .
C22 C 0.1574(3) -0.0683(3) 0.8856(2) 0.0556(8) Uani 1 1 d . . . . .
H22 H 0.108619 -0.111312 0.910740 0.067 Uiso 1 1 calc R U . . .
C32 C 0.3133(3) 0.1885(2) 0.47789(18) 0.0481(7) Uani 1 1 d . . . . .
C20 C 0.3439(3) -0.0471(2) 0.8055(2) 0.0506(7) Uani 1 1 d . . . . .
H20 H 0.422376 -0.076616 0.775581 0.061 Uiso 1 1 calc R U . . .
C33 C 0.2913(3) 0.1407(2) 0.40989(19) 0.0489(7) Uani 1 1 d . . . . .
H33 H 0.253976 0.086567 0.421441 0.059 Uiso 1 1 calc R U . . .
C7 C 0.4169(3) 0.4069(3) 0.65661(17) 0.0465(7) Uani 1 1 d . . . . .
H7 H 0.369589 0.358046 0.647527 0.056 Uiso 1 1 calc R U . . .
C21 C 0.2730(3) -0.1105(3) 0.8415(3) 0.0611(9) Uani 1 1 d . . . . .
H21 H 0.302933 -0.182086 0.836141 0.073 Uiso 1 1 calc R U . . .
C34 C 0.3233(3) 0.1708(3) 0.3243(2) 0.0546(8) Uani 1 1 d . . . . .
H34 H 0.307765 0.136477 0.278678 0.066 Uiso 1 1 calc R U . . .
C35 C 0.3760(4) 0.2479(3) 0.3054(2) 0.0614(9) Uani 1 1 d . . . . .
H35 H 0.399338 0.266896 0.247188 0.074 Uiso 1 1 calc R U . . .
C26 C 0.2369(3) 0.0361(3) 0.59192(19) 0.0577(9) Uani 1 1 d . . . . .
C18 C 0.6761(3) 0.0728(3) 0.7474(3) 0.0575(9) Uani 1 1 d . . . . .
H18 H 0.673062 0.098588 0.688612 0.069 Uiso 1 1 calc R U . . .
C15 C 0.6927(3) -0.0029(3) 0.9188(3) 0.0667(10) Uani 1 1 d . . . . .
H15 H 0.697376 -0.028035 0.977633 0.080 Uiso 1 1 calc R U . . .
C12 C 0.1906(4) 0.3156(3) 0.9911(3) 0.0694(11) Uani 1 1 d . . . . .
H12A H 0.171206 0.376306 1.024031 0.104 Uiso 1 1 calc R U . . .
H12B H 0.162374 0.261899 1.025772 0.104 Uiso 1 1 calc R U . . .
H12C H 0.148249 0.333104 0.937692 0.104 Uiso 1 1 calc R U . . .
C8 C 0.5526(3) 0.3603(3) 0.6214(2) 0.0652(10) Uani 1 1 d . . . . .
H8A H 0.555408 0.350125 0.559888 0.098 Uiso 1 1 calc R U . . .
H8B H 0.587269 0.294473 0.653065 0.098 Uiso 1 1 calc R U . . .
H8C H 0.601594 0.406710 0.628849 0.098 Uiso 1 1 calc R U . . .
C16 C 0.7993(3) -0.0108(3) 0.8658(4) 0.0746(12) Uani 1 1 d . . . . .
H16 H 0.878035 -0.042066 0.887680 0.090 Uiso 1 1 calc R U . . .
C17 C 0.7929(3) 0.0261(3) 0.7815(3) 0.0725(12) Uani 1 1 d . . . . .
H17 H 0.867469 0.020496 0.745125 0.087 Uiso 1 1 calc R U . . .
C41 C 0.0935(11) 0.5764(9) 0.8459(8) 0.073(3) Uani 0.716(12) 1 d . . P A 1
H41A H 0.180779 0.533404 0.847710 0.088 Uiso 0.716(12) 1 calc R U P A 1
H41B H 0.047752 0.567122 0.902499 0.088 Uiso 0.716(12) 1 calc R U P A 1
C27 C 0.3263(4) -0.0534(3) 0.5655(3) 0.0701(10) Uani 1 1 d . . . . .
H27 H 0.409380 -0.052081 0.548761 0.084 Uiso 1 1 calc R U . . .
C42 C -0.1680(10) 0.3959(6) 0.8842(6) 0.076(3) Uani 0.716(12) 1 d . . P A 1
H42A H -0.226405 0.461839 0.865212 0.091 Uiso 0.716(12) 1 calc R U P A 1
H42B H -0.105170 0.410100 0.916891 0.091 Uiso 0.716(12) 1 calc R U P A 1
C36 C 0.3951(5) 0.2980(4) 0.3722(2) 0.0930(16) Uani 1 1 d . . . . .
H36 H 0.429823 0.353594 0.360031 0.112 Uiso 1 1 calc R U . . .
C11 C 0.4013(5) 0.2530(3) 1.0505(2) 0.0796(13) Uani 1 1 d . . . . .
H11A H 0.491268 0.231795 1.034846 0.119 Uiso 1 1 calc R U . . .
H11B H 0.377379 0.197699 1.085980 0.119 Uiso 1 1 calc R U . . .
H11C H 0.379361 0.314039 1.083238 0.119 Uiso 1 1 calc R U . . .
C45 C -0.1646(6) 0.2578(6) 0.8113(4) 0.0545(18) Uani 0.716(12) 1 d . . P A 1
H45A H -0.100871 0.191116 0.819498 0.065 Uiso 0.716(12) 1 calc R U P A 1
H45B H -0.199427 0.260365 0.755318 0.065 Uiso 0.716(12) 1 calc R U P A 1
C9 C 0.3577(4) 0.5073(3) 0.6065(2) 0.0722(11) Uani 1 1 d . . . . .
H9A H 0.270081 0.533239 0.627873 0.108 Uiso 1 1 calc R U . . .
H9B H 0.363407 0.495997 0.544950 0.108 Uiso 1 1 calc R U . . .
H9C H 0.401674 0.557214 0.614292 0.108 Uiso 1 1 calc R U . . .
C37 C 0.3642(5) 0.2685(4) 0.4570(2) 0.0874(15) Uani 1 1 d . . . . .
H37 H 0.378510 0.304330 0.502006 0.105 Uiso 1 1 calc R U . . .
C28 C 0.2953(6) -0.1432(3) 0.5634(3) 0.0884(14) Uani 1 1 d . . . . .
H28 H 0.356559 -0.203447 0.546127 0.106 Uiso 1 1 calc R U . . .
C39 C -0.0137(15) 0.7251(10) 0.7657(11) 0.119(5) Uani 0.716(12) 1 d . . P A 1
H39A H -0.082351 0.780336 0.791243 0.143 Uiso 0.716(12) 1 calc R U P A 1
H39B H 0.018698 0.751689 0.709580 0.143 Uiso 0.716(12) 1 calc R U P A 1
C40 C 0.0890(11) 0.6846(8) 0.8265(10) 0.113(4) Uani 0.716(12) 1 d . . P A 1
H40A H 0.169512 0.691189 0.798226 0.135 Uiso 0.716(12) 1 calc R U P A 1
H40B H 0.068819 0.721804 0.879816 0.135 Uiso 0.716(12) 1 calc R U P A 1
C44 C -0.2634(8) 0.2688(7) 0.8816(8) 0.093(3) Uani 0.716(12) 1 d . . P A 1
H44A H -0.345742 0.301588 0.859332 0.111 Uiso 0.716(12) 1 calc R U P A 1
H44B H -0.263380 0.201285 0.910457 0.111 Uiso 0.716(12) 1 calc R U P A 1
C31 C 0.1178(5) 0.0318(4) 0.6151(4) 0.116(2) Uani 1 1 d . . . . .
H31 H 0.056496 0.090642 0.635040 0.140 Uiso 1 1 calc R U . . .
C29 C 0.1748(7) -0.1440(5) 0.5865(4) 0.127(3) Uani 1 1 d . . . . .
H29 H 0.153637 -0.205980 0.586145 0.152 Uiso 1 1 calc R U . . .
C43 C -0.2375(10) 0.3312(6) 0.9402(5) 0.087(2) Uani 0.716(12) 1 d . . P A 1
H43A H -0.185600 0.288995 0.985169 0.105 Uiso 0.716(12) 1 calc R U P A 1
H43B H -0.315409 0.374313 0.968637 0.105 Uiso 0.716(12) 1 calc R U P A 1
C30 C 0.0848(7) -0.0584(6) 0.6100(5) 0.164(4) Uani 1 1 d . . . . .
H30 H 0.000914 -0.059507 0.622704 0.197 Uiso 1 1 calc R U . . .
C38 C -0.0555(8) 0.6379(5) 0.7552(6) 0.091(3) Uani 0.716(12) 1 d . . P A 1
H38A H -0.133918 0.641314 0.791728 0.109 Uiso 0.716(12) 1 calc R U P A 1
H38B H -0.071064 0.636639 0.694212 0.109 Uiso 0.716(12) 1 calc R U P A 1
N2 N -0.0561(4) 0.4097(4) 0.5804(3) 0.1051(14) Uani 1 1 d . . . . .
C46 C -0.1709(5) 0.4742(6) 0.6213(4) 0.118(2) Uani 1 1 d . . . . .
H46A H -0.235506 0.492741 0.580605 0.177 Uiso 1 1 calc R U . . .
H46B H -0.156086 0.536305 0.638010 0.177 Uiso 1 1 calc R U . . .
H46C H -0.198212 0.436906 0.672826 0.177 Uiso 1 1 calc R U . . .
C48 C -0.0188(6) 0.4540(6) 0.4939(4) 0.135(3) Uani 1 1 d . . . . .
H48A H 0.051482 0.403106 0.464788 0.162 Uiso 1 1 calc R U . . .
H48B H -0.089442 0.472496 0.457156 0.162 Uiso 1 1 calc R U . . .
C47 C -0.0836(6) 0.3143(6) 0.5627(4) 0.131(2) Uani 1 1 d . . . . .
H47A H -0.102809 0.278295 0.617493 0.196 Uiso 1 1 calc R U . . .
H47B H -0.010993 0.270243 0.531055 0.196 Uiso 1 1 calc R U . . .
H47C H -0.155212 0.331541 0.527968 0.196 Uiso 1 1 calc R U . . .
C38A C 0.0016(18) 0.6580(10) 0.7089(12) 0.077(5) Uiso 0.284(12) 1 d D . P A 2
H38C H -0.079974 0.661577 0.688804 0.092 Uiso 0.284(12) 1 calc R U P A 2
H38D H 0.057691 0.671192 0.658607 0.092 Uiso 0.284(12) 1 calc R U P A 2
O1A O 0.0559(17) 0.5585(12) 0.7542(10) 0.054(4) Uiso 0.284(12) 1 d D . P A 2
C43A C -0.1850(16) 0.3252(11) 0.9542(10) 0.055(4) Uiso 0.284(12) 1 d D . P A 2
H43C H -0.108279 0.287381 0.982030 0.066 Uiso 0.284(12) 1 calc R U P A 2
H43D H -0.250164 0.355258 0.999684 0.066 Uiso 0.284(12) 1 calc R U P A 2
O2A O -0.0854(17) 0.3307(15) 0.8321(12) 0.066(6) Uiso 0.284(12) 1 d D . P A 2
C44A C -0.229(2) 0.2525(16) 0.9037(14) 0.067(6) Uiso 0.284(12) 1 d D . P A 2
H44C H -0.320631 0.269822 0.906726 0.080 Uiso 0.284(12) 1 calc R U P A 2
H44D H -0.193975 0.180095 0.924186 0.080 Uiso 0.284(12) 1 calc R U P A 2
C39A C -0.014(2) 0.735(2) 0.7781(18) 0.061(6) Uiso 0.284(12) 1 d D . P A 2
H39C H -0.080929 0.733039 0.824005 0.073 Uiso 0.284(12) 1 calc R U P A 2
H39D H -0.022957 0.805937 0.753410 0.073 Uiso 0.284(12) 1 calc R U P A 2
C42A C -0.159(3) 0.4105(13) 0.8883(12) 0.062(7) Uiso 0.284(12) 1 d D . P A 2
H42C H -0.234880 0.455958 0.863273 0.075 Uiso 0.284(12) 1 calc R U P A 2
H42D H -0.110326 0.450463 0.910095 0.075 Uiso 0.284(12) 1 calc R U P A 2
C40A C 0.118(2) 0.6805(17) 0.8070(17) 0.068(6) Uiso 0.284(12) 1 d D . P A 2
H40C H 0.183408 0.682346 0.759276 0.081 Uiso 0.284(12) 1 calc R U P A 2
H40D H 0.135239 0.711827 0.857130 0.081 Uiso 0.284(12) 1 calc R U P A 2
C45A C -0.172(3) 0.276(3) 0.8116(16) 0.156(19) Uiso 0.284(12) 1 d D . P A 2
H45C H -0.128218 0.213093 0.782615 0.187 Uiso 0.284(12) 1 calc R U P A 2
H45D H -0.236643 0.320244 0.775087 0.187 Uiso 0.284(12) 1 calc R U P A 2
C41A C 0.112(2) 0.5699(17) 0.8318(13) 0.044(5) Uiso 0.284(12) 1 d D . P A 2
H41C H 0.195663 0.520663 0.836913 0.053 Uiso 0.284(12) 1 calc R U P A 2
H41D H 0.058080 0.564801 0.885478 0.053 Uiso 0.284(12) 1 calc R U P A 2


_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
K001 O2A 2.68(2) . ?
K001 O2 2.711(5) . ?
K001 O1 2.710(6) . ?
K001 O1A 2.714(17) . ?
K001 N1 2.750(2) . ?
K001 N2 2.975(4) . ?
K001 C1 3.386(3) . ?
K001 C41A 3.51(2) . ?
K001 P1 3.5105(16) . ?
K001 Si1 3.8075(17) . ?
Si1 N1 1.653(2) . ?
Si1 C19 1.896(3) . ?
Si1 C13 1.905(3) . ?
Si1 C25 1.913(3) . ?
P1 C25 1.846(3) . ?
P1 C26 1.850(4) . ?
P1 C32 1.858(3) . ?
N1 C1 1.373(3) . ?
O2 C42 1.428(7) . ?
O2 C45 1.448(7) . ?
C1 C2 1.436(4) . ?
C1 C6 1.438(3) . ?
C6 C5 1.390(4) . ?
C6 C10 1.515(4) . ?
O1 C41 1.395(9) . ?
O1 C38 1.404(8) . ?
C13 C14 1.401(4) . ?
C13 C18 1.411(4) . ?
C19 C20 1.405(4) . ?
C19 C24 1.407(4) . ?
C5 C4 1.392(4) . ?
C14 C15 1.390(4) . ?
C24 C23 1.399(4) . ?
C2 C3 1.397(4) . ?
C2 C7 1.518(4) . ?
C23 C22 1.374(5) . ?
C10 C11 1.527(4) . ?
C10 C12 1.543(5) . ?
C4 C3 1.386(4) . ?
C22 C21 1.395(5) . ?
C32 C37 1.379(5) . ?
C32 C33 1.383(4) . ?
C20 C21 1.388(4) . ?
C33 C34 1.399(5) . ?
C7 C9 1.522(5) . ?
C7 C8 1.537(5) . ?
C34 C35 1.353(5) . ?
C35 C36 1.374(5) . ?
C26 C31 1.370(6) . ?
C26 C27 1.407(5) . ?
C18 C17 1.421(6) . ?
C15 C16 1.365(6) . ?
C16 C17 1.364(6) . ?
C41 C40 1.473(10) . ?
C27 C28 1.381(5) . ?
C42 C43 1.508(9) . ?
C36 C37 1.382(5) . ?
C45 C44 1.462(9) . ?
C28 C29 1.370(8) . ?
C39 C38 1.439(15) . ?
C39 C40 1.519(14) . ?
C44 C43 1.420(11) . ?
C31 C30 1.405(7) . ?
C29 C30 1.359(9) . ?
N2 C46 1.458(7) . ?
N2 C47 1.489(8) . ?
N2 C48 1.495(8) . ?
C48 C48 1.482(13) 2_566 ?
C38A O1A 1.468(5) . ?
C38A C39A 1.549(5) . ?
O1A C41A 1.470(5) . ?
C43A C44A 1.547(5) . ?
C43A C42A 1.551(5) . ?
O2A C42A 1.470(5) . ?
O2A C45A 1.472(5) . ?
C44A C45A 1.551(5) . ?
C39A C40A 1.551(5) . ?
C40A C41A 1.550(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 K001 O1 85.6(2) . . ?
O2A K001 O1A 93.9(5) . . ?
O2A K001 N1 115.0(4) . . ?
O2 K001 N1 123.57(19) . . ?
O1 K001 N1 106.24(16) . . ?
O1A K001 N1 106.3(4) . . ?
O2A K001 N2 89.1(4) . . ?
O2 K001 N2 80.1(2) . . ?
O1 K001 N2 95.1(2) . . ?
O1A K001 N2 91.0(4) . . ?
N1 K001 N2 148.57(10) . . ?
O2A K001 C1 118.1(4) . . ?
O2 K001 C1 127.00(18) . . ?
O1 K001 C1 83.62(16) . . ?
O1A K001 C1 83.2(4) . . ?
N1 K001 C1 23.01(6) . . ?
N2 K001 C1 152.47(10) . . ?
O2A K001 C41A 91.7(6) . . ?
O1A K001 C41A 23.1(3) . . ?
N1 K001 C41A 86.5(4) . . ?
N2 K001 C41A 114.0(4) . . ?
C1 K001 C41A 64.1(4) . . ?
O2A K001 P1 117.9(4) . . ?
O2 K001 P1 116.47(11) . . ?
O1 K001 P1 156.2(2) . . ?
O1A K001 P1 146.9(3) . . ?
N1 K001 P1 69.98(5) . . ?
N2 K001 P1 81.15(10) . . ?
C1 K001 P1 89.04(5) . . ?
C41A K001 P1 147.6(4) . . ?
O2A K001 Si1 111.4(4) . . ?
O2 K001 Si1 118.05(17) . . ?
O1 K001 Si1 128.88(15) . . ?
O1A K001 Si1 128.6(4) . . ?
N1 K001 Si1 22.65(5) . . ?
N2 K001 Si1 131.34(11) . . ?
C1 K001 Si1 45.50(5) . . ?
C41A K001 Si1 109.1(4) . . ?
P1 K001 Si1 50.19(3) . . ?
N1 Si1 C19 110.88(12) . . ?
N1 Si1 C13 116.24(12) . . ?
C19 Si1 C13 105.87(12) . . ?
N1 Si1 C25 112.85(13) . . ?
C19 Si1 C25 104.88(12) . . ?
C13 Si1 C25 105.25(13) . . ?
N1 Si1 K001 39.83(8) . . ?
C19 Si1 K001 88.69(9) . . ?
C13 Si1 K001 156.05(8) . . ?
C25 Si1 K001 88.69(10) . . ?
C25 P1 C26 103.03(16) . . ?
C25 P1 C32 102.62(14) . . ?
C26 P1 C32 101.71(14) . . ?
C25 P1 K001 99.29(9) . . ?
C26 P1 K001 125.91(11) . . ?
C32 P1 K001 120.43(11) . . ?
C1 N1 Si1 136.05(18) . . ?
C1 N1 K001 105.47(15) . . ?
Si1 N1 K001 117.53(10) . . ?
C42 O2 C45 106.0(5) . . ?
C42 O2 K001 123.6(5) . . ?
C45 O2 K001 128.2(4) . . ?
N1 C1 C2 121.3(2) . . ?
N1 C1 C6 121.9(2) . . ?
C2 C1 C6 116.7(2) . . ?
N1 C1 K001 51.52(12) . . ?
C2 C1 K001 95.84(16) . . ?
C6 C1 K001 119.91(16) . . ?
C5 C6 C1 120.4(2) . . ?
C5 C6 C10 120.2(2) . . ?
C1 C6 C10 119.3(2) . . ?
C41 O1 C38 105.9(7) . . ?
C41 O1 K001 122.4(6) . . ?
C38 O1 K001 131.7(6) . . ?
P1 C25 Si1 111.90(15) . . ?
C14 C13 C18 116.4(3) . . ?
C14 C13 Si1 120.2(2) . . ?
C18 C13 Si1 123.4(3) . . ?
C20 C19 C24 116.3(3) . . ?
C20 C19 Si1 120.9(2) . . ?
C24 C19 Si1 122.7(2) . . ?
C6 C5 C4 122.1(3) . . ?
C15 C14 C13 122.5(3) . . ?
C23 C24 C19 121.7(3) . . ?
C3 C2 C1 120.5(2) . . ?
C3 C2 C7 119.8(3) . . ?
C1 C2 C7 119.7(2) . . ?
C22 C23 C24 120.1(3) . . ?
C6 C10 C11 114.4(3) . . ?
C6 C10 C12 110.1(3) . . ?
C11 C10 C12 110.6(3) . . ?
C3 C4 C5 118.5(3) . . ?
C4 C3 C2 121.9(3) . . ?
C23 C22 C21 120.0(3) . . ?
C37 C32 C33 116.8(3) . . ?
C37 C32 P1 117.5(2) . . ?
C33 C32 P1 125.5(3) . . ?
C21 C20 C19 122.3(3) . . ?
C32 C33 C34 120.9(3) . . ?
C9 C7 C2 113.6(3) . . ?
C9 C7 C8 111.1(3) . . ?
C2 C7 C8 109.9(3) . . ?
C20 C21 C22 119.6(3) . . ?
C35 C34 C33 121.2(3) . . ?
C34 C35 C36 118.5(3) . . ?
C31 C26 C27 117.9(4) . . ?
C31 C26 P1 118.4(3) . . ?
C27 C26 P1 123.7(3) . . ?
C13 C18 C17 120.0(4) . . ?
C16 C15 C14 120.1(4) . . ?
C15 C16 C17 120.1(3) . . ?
C16 C17 C18 120.9(3) . . ?
O1 C41 C40 106.6(9) . . ?
C28 C27 C26 121.1(4) . . ?
O2 C42 C43 107.4(6) . . ?
C35 C36 C37 120.7(4) . . ?
O2 C45 C44 108.6(5) . . ?
C32 C37 C36 121.8(3) . . ?
C29 C28 C27 119.0(5) . . ?
C38 C39 C40 104.3(9) . . ?
C41 C40 C39 104.1(9) . . ?
C43 C44 C45 106.0(6) . . ?
C26 C31 C30 121.1(5) . . ?
C30 C29 C28 121.7(5) . . ?
C44 C43 C42 104.1(7) . . ?
C29 C30 C31 119.0(6) . . ?
O1 C38 C39 108.0(8) . . ?
C46 N2 C47 106.2(5) . . ?
C46 N2 C48 113.0(5) . . ?
C47 N2 C48 105.1(5) . . ?
C46 N2 K001 101.4(3) . . ?
C47 N2 K001 107.3(4) . . ?
C48 N2 K001 122.8(3) . . ?
C48 C48 N2 108.6(7) 2_566 . ?
O1A C38A C39A 103.7(18) . . ?
C38A O1A C41A 111.3(17) . . ?
C38A O1A K001 137.8(12) . . ?
C41A O1A K001 110.3(11) . . ?
C44A C43A C42A 107.3(16) . . ?
C42A O2A C45A 106(2) . . ?
C42A O2A K001 121.2(14) . . ?
C45A O2A K001 124.7(14) . . ?
C43A C44A C45A 99.6(16) . . ?
C38A C39A C40A 91.8(16) . . ?
O2A C42A C43A 88.6(14) . . ?
C41A C40A C39A 103(2) . . ?
O2A C45A C44A 100.4(18) . . ?
O1A C41A C40A 96.5(17) . . ?
O1A C41A K001 46.5(9) . . ?
C40A C41A K001 137.6(14) . . ?

_refine_diff_density_max         0.588
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.064



#===END
####################################################################### 
# 
# 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_compound_1b
_database_code_depnum_ccdc_archive 'CCDC 2057297'
loop_
_audit_author_name
_audit_author_address
'Terrance Hadlington'
;TU Munich
Germany
;
_audit_update_record             
;
2021-01-19 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H46 Cl Ge N P Si'
_chemical_formula_sum            'C34 H46 Cl Ge N P Si'
_chemical_formula_weight         635.82

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

_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                   15.550(3)
_cell_length_b                   19.910(4)
_cell_length_c                   21.820(4)
_cell_angle_alpha                90
_cell_angle_beta                 95.60(3)
_cell_angle_gamma                90
_cell_volume                     6723(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2000
_cell_measurement_theta_min      1.92
_cell_measurement_theta_max      32.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless

_exptl_crystal_density_diffrn    1.256
_exptl_crystal_F_000             2680
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.22
_exptl_absorpt_coefficient_mu    1.097
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.680
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'STOE X-AREA 1.76'

_diffrn_ambient_temperature      150(2)
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            76019
_diffrn_reflns_av_unetI/netI     0.1091
_diffrn_reflns_av_R_equivalents  0.1118
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.561
_diffrn_reflns_theta_max         27.498
_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             15430
_reflns_number_gt                8305
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0419P)²+3.4583P] 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         15430
_refine_ls_number_parameters     719
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1437
_refine_ls_R_factor_gt           0.0570
_refine_ls_wR_factor_ref         0.1237
_refine_ls_wR_factor_gt          0.0974
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_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
Ge1 Ge 0.56501(3) 0.77382(2) 0.12139(2) 0.02338(11) Uani 1 1 d . . . . .
Ge2 Ge 0.33840(3) 0.78788(2) 0.57513(2) 0.02598(12) Uani 1 1 d . . . . .
Cl1 Cl 0.53395(7) 0.88937(5) 0.12629(5) 0.0322(2) Uani 1 1 d . . . . .
P1 P 0.53382(7) 0.76952(5) 0.23024(5) 0.0231(2) Uani 1 1 d . . . . .
P2 P 0.37455(7) 0.78949(5) 0.46780(5) 0.0262(2) Uani 1 1 d . . . . .
Si1 Si 0.72632(7) 0.79621(5) 0.22737(5) 0.0241(3) Uani 1 1 d . . . . .
Cl2 Cl 0.36431(8) 0.90376(5) 0.57709(6) 0.0431(3) Uani 1 1 d . . . . .
Si2 Si 0.18024(8) 0.81387(5) 0.46768(6) 0.0279(3) Uani 1 1 d . . . . .
N1 N 0.6849(2) 0.77321(15) 0.15317(14) 0.0234(7) Uani 1 1 d . . . . .
N2 N 0.2201(2) 0.78696(15) 0.54106(15) 0.0245(8) Uani 1 1 d . . . . .
C26 C 0.4330(3) 0.80699(19) 0.24962(18) 0.0259(9) Uani 1 1 d . . . . .
C41 C 0.2156(3) 0.63729(19) 0.54930(19) 0.0294(10) Uani 1 1 d . . . . .
H41 H 0.247442 0.666115 0.521558 0.035 Uiso 1 1 calc R U . . .
C1 C 0.7377(3) 0.74378(19) 0.10831(19) 0.0255(9) Uani 1 1 d . . . . .
C6 C 0.7446(3) 0.67330(19) 0.10273(18) 0.0256(9) Uani 1 1 d . . . . .
C10 C 0.6928(3) 0.62405(19) 0.13832(19) 0.0283(10) Uani 1 1 d . . . . .
H10 H 0.663411 0.650327 0.169331 0.034 Uiso 1 1 calc R U . . .
C19 C 0.6253(3) 0.81562(19) 0.26633(18) 0.0267(9) Uani 1 1 d . . . . .
H19A H 0.634733 0.803348 0.310438 0.032 Uiso 1 1 calc R U . . .
H19B H 0.613111 0.864394 0.263576 0.032 Uiso 1 1 calc R U . . .
C32 C 0.1652(3) 0.75376(19) 0.58228(18) 0.0250(9) Uani 1 1 d . . . . .
C20 C 0.5373(3) 0.68363(19) 0.25917(19) 0.0257(9) Uani 1 1 d . . . . .
C37 C 0.1594(3) 0.68295(19) 0.58408(18) 0.0273(9) Uani 1 1 d . . . . .
C57 C 0.4737(3) 0.8295(2) 0.44921(18) 0.0313(10) Uani 1 1 d . . . . .
C51 C 0.3765(3) 0.70440(19) 0.43843(18) 0.0272(9) Uani 1 1 d . . . . .
C33 C 0.1196(3) 0.7931(2) 0.62295(19) 0.0292(10) Uani 1 1 d . . . . .
C36 C 0.1024(3) 0.6531(2) 0.6218(2) 0.0318(10) Uani 1 1 d . . . . .
H36 H 0.096633 0.605641 0.621758 0.038 Uiso 1 1 calc R U . . .
C21 C 0.5726(3) 0.6675(2) 0.3190(2) 0.0334(11) Uani 1 1 d . . . . .
H21 H 0.594252 0.702112 0.346312 0.040 Uiso 1 1 calc R U . . .
C31 C 0.3556(3) 0.7730(2) 0.23401(18) 0.0304(10) Uani 1 1 d . . . . .
H31 H 0.356698 0.728450 0.218444 0.036 Uiso 1 1 calc R U . . .
C13 C 0.7887(3) 0.7244(2) 0.26862(18) 0.0275(9) Uani 1 1 d . . . . .
H13 H 0.754772 0.682697 0.257599 0.033 Uiso 1 1 calc R U . . .
C58 C 0.5494(3) 0.7923(2) 0.45073(19) 0.0329(10) Uani 1 1 d . . . . .
H58 H 0.548248 0.745288 0.458222 0.040 Uiso 1 1 calc R U . . .
C25 C 0.5031(3) 0.6325(2) 0.2207(2) 0.0336(10) Uani 1 1 d . . . . .
H25 H 0.478124 0.642817 0.180302 0.040 Uiso 1 1 calc R U . . .
C52 C 0.4108(3) 0.6536(2) 0.4768(2) 0.0336(10) Uani 1 1 d . . . . .
H52 H 0.433280 0.664110 0.517697 0.040 Uiso 1 1 calc R U . . .
C50 C 0.2826(3) 0.8334(2) 0.4301(2) 0.0327(10) Uani 1 1 d . . . . .
H50A H 0.274632 0.820112 0.386168 0.039 Uiso 1 1 calc R U . . .
H50B H 0.293657 0.882347 0.432010 0.039 Uiso 1 1 calc R U . . .
C16 C 0.7942(3) 0.8762(2) 0.2309(2) 0.0329(10) Uani 1 1 d . . . . .
H16 H 0.836945 0.871452 0.199780 0.040 Uiso 1 1 calc R U . . .
C38 C 0.1332(3) 0.8680(2) 0.6304(2) 0.0345(11) Uani 1 1 d . . . . .
H38 H 0.164806 0.884103 0.595393 0.041 Uiso 1 1 calc R U . . .
C2 C 0.7784(3) 0.7857(2) 0.06785(19) 0.0306(10) Uani 1 1 d . . . . .
C7 C 0.7638(3) 0.8611(2) 0.0645(2) 0.0345(11) Uani 1 1 d . . . . .
H7 H 0.734757 0.874530 0.101508 0.041 Uiso 1 1 calc R U . . .
C34 C 0.0644(3) 0.7601(2) 0.6603(2) 0.0379(11) Uani 1 1 d . . . . .
H34 H 0.033083 0.785926 0.687284 0.045 Uiso 1 1 calc R U . . .
C23 C 0.5424(3) 0.5505(2) 0.2994(2) 0.0435(12) Uani 1 1 d . . . . .
H23 H 0.545076 0.505108 0.312973 0.052 Uiso 1 1 calc R U . . .
C5 C 0.7986(3) 0.6468(2) 0.0611(2) 0.0376(11) Uani 1 1 d . . . . .
H5 H 0.804917 0.599468 0.058066 0.045 Uiso 1 1 calc R U . . .
C43 C 0.1636(3) 0.5851(2) 0.5088(2) 0.0408(12) Uani 1 1 d . . . . .
H43A H 0.138662 0.551971 0.535164 0.061 Uiso 1 1 calc R U . . .
H43B H 0.202045 0.562389 0.482406 0.061 Uiso 1 1 calc R U . . .
H43C H 0.117203 0.607767 0.483120 0.061 Uiso 1 1 calc R U . . .
C44 C 0.1171(3) 0.7448(2) 0.42451(19) 0.0320(10) Uani 1 1 d . . . . .
H44 H 0.148875 0.702326 0.436200 0.038 Uiso 1 1 calc R U . . .
C24 C 0.5054(3) 0.5661(2) 0.2413(2) 0.0414(12) Uani 1 1 d . . . . .
H24 H 0.481325 0.531481 0.214974 0.050 Uiso 1 1 calc R U . . .
C56 C 0.3427(3) 0.6875(2) 0.3782(2) 0.0377(11) Uani 1 1 d . . . . .
H56 H 0.319040 0.721383 0.350881 0.045 Uiso 1 1 calc R U . . .
C53 C 0.4130(3) 0.5876(2) 0.4566(2) 0.0395(12) Uani 1 1 d . . . . .
H53 H 0.437676 0.553537 0.483268 0.047 Uiso 1 1 calc R U . . .
C54 C 0.3795(3) 0.5716(2) 0.3978(2) 0.0481(13) Uani 1 1 d . . . . .
H54 H 0.380647 0.526466 0.383815 0.058 Uiso 1 1 calc R U . . .
C35 C 0.0543(3) 0.6910(2) 0.6589(2) 0.0389(11) Uani 1 1 d . . . . .
H35 H 0.014775 0.669878 0.683321 0.047 Uiso 1 1 calc R U . . .
C14 C 0.7989(3) 0.7277(2) 0.33923(19) 0.0345(10) Uani 1 1 d . . . . .
H14A H 0.824574 0.685752 0.355845 0.052 Uiso 1 1 calc R U . . .
H14B H 0.742077 0.734002 0.354274 0.052 Uiso 1 1 calc R U . . .
H14C H 0.836529 0.765469 0.352653 0.052 Uiso 1 1 calc R U . . .
C30 C 0.2773(3) 0.8036(2) 0.24100(19) 0.0374(11) Uani 1 1 d . . . . .
H30 H 0.224828 0.780298 0.229687 0.045 Uiso 1 1 calc R U . . .
C11 C 0.6229(3) 0.5891(2) 0.09566(19) 0.0352(11) Uani 1 1 d . . . . .
H11A H 0.583938 0.622849 0.075458 0.053 Uiso 1 1 calc R U . . .
H11B H 0.589918 0.558617 0.119760 0.053 Uiso 1 1 calc R U . . .
H11C H 0.649977 0.563425 0.064393 0.053 Uiso 1 1 calc R U . . .
C42 C 0.2832(3) 0.6013(2) 0.5941(2) 0.0344(11) Uani 1 1 d . . . . .
H42A H 0.320424 0.634642 0.616422 0.052 Uiso 1 1 calc R U . . .
H42B H 0.318383 0.571601 0.570802 0.052 Uiso 1 1 calc R U . . .
H42C H 0.253686 0.574591 0.623453 0.052 Uiso 1 1 calc R U . . .
C17 C 0.8459(3) 0.8876(2) 0.2939(2) 0.0491(14) Uani 1 1 d . . . . .
H17A H 0.873883 0.931694 0.294402 0.074 Uiso 1 1 calc R U . . .
H17B H 0.889983 0.852529 0.301066 0.074 Uiso 1 1 calc R U . . .
H17C H 0.806687 0.885721 0.326444 0.074 Uiso 1 1 calc R U . . .
C29 C 0.2755(3) 0.8675(2) 0.2643(2) 0.0445(13) Uani 1 1 d . . . . .
H29 H 0.221684 0.888612 0.268835 0.053 Uiso 1 1 calc R U . . .
C60 C 0.6290(3) 0.8920(3) 0.4298(2) 0.0485(14) Uani 1 1 d . . . . .
H60 H 0.682068 0.913331 0.423557 0.058 Uiso 1 1 calc R U . . .
C27 C 0.4303(3) 0.8717(2) 0.2737(2) 0.0407(12) Uani 1 1 d . . . . .
H27 H 0.482400 0.895432 0.285114 0.049 Uiso 1 1 calc R U . . .
C18 C 0.7405(3) 0.9395(2) 0.2139(2) 0.0428(12) Uani 1 1 d . . . . .
H18A H 0.706963 0.951498 0.248025 0.064 Uiso 1 1 calc R U . . .
H18B H 0.701157 0.930733 0.176889 0.064 Uiso 1 1 calc R U . . .
H18C H 0.779257 0.976644 0.205897 0.064 Uiso 1 1 calc R U . . .
C47 C 0.1134(3) 0.8937(2) 0.4656(2) 0.0416(12) Uani 1 1 d . . . . .
H47 H 0.067051 0.886630 0.493662 0.050 Uiso 1 1 calc R U . . .
C15 C 0.8778(3) 0.7143(2) 0.2441(2) 0.0383(11) Uani 1 1 d . . . . .
H15A H 0.915682 0.752069 0.257083 0.057 Uiso 1 1 calc R U . . .
H15B H 0.870570 0.711909 0.199059 0.057 Uiso 1 1 calc R U . . .
H15C H 0.903755 0.672378 0.260730 0.057 Uiso 1 1 calc R U . . .
C59 C 0.6274(3) 0.8238(3) 0.4412(2) 0.0427(12) Uani 1 1 d . . . . .
H59 H 0.679228 0.798322 0.442659 0.051 Uiso 1 1 calc R U . . .
C62 C 0.4769(3) 0.8985(2) 0.4376(2) 0.0449(13) Uani 1 1 d . . . . .
H62 H 0.425579 0.924563 0.436530 0.054 Uiso 1 1 calc R U . . .
C12 C 0.7513(3) 0.5720(2) 0.1732(2) 0.0427(12) Uani 1 1 d . . . . .
H12A H 0.773342 0.540764 0.143729 0.064 Uiso 1 1 calc R U . . .
H12B H 0.718082 0.547073 0.201611 0.064 Uiso 1 1 calc R U . . .
H12C H 0.799801 0.594873 0.196454 0.064 Uiso 1 1 calc R U . . .
C8 C 0.7019(3) 0.8783(2) 0.0070(2) 0.0429(12) Uani 1 1 d . . . . .
H8A H 0.727038 0.862945 -0.030050 0.064 Uiso 1 1 calc R U . . .
H8B H 0.692926 0.926961 0.004749 0.064 Uiso 1 1 calc R U . . .
H8C H 0.646317 0.855775 0.009708 0.064 Uiso 1 1 calc R U . . .
C4 C 0.8429(3) 0.6882(2) 0.0245(2) 0.0445(13) Uani 1 1 d . . . . .
H4 H 0.880892 0.669578 -0.002554 0.053 Uiso 1 1 calc R U . . .
C22 C 0.5760(3) 0.6017(2) 0.3382(2) 0.0433(12) Uani 1 1 d . . . . .
H22 H 0.601434 0.591073 0.378415 0.052 Uiso 1 1 calc R U . . .
C3 C 0.8317(3) 0.7567(2) 0.0272(2) 0.0409(12) Uani 1 1 d . . . . .
H3 H 0.860819 0.784860 0.000810 0.049 Uiso 1 1 calc R U . . .
C46 C 0.1098(3) 0.7473(2) 0.3534(2) 0.0458(13) Uani 1 1 d . . . . .
H46A H 0.081914 0.706138 0.336706 0.069 Uiso 1 1 calc R U . . .
H46B H 0.167654 0.750939 0.339500 0.069 Uiso 1 1 calc R U . . .
H46C H 0.075151 0.786290 0.338914 0.069 Uiso 1 1 calc R U . . .
C61 C 0.5545(3) 0.9293(3) 0.4275(2) 0.0491(14) Uani 1 1 d . . . . .
H61 H 0.555942 0.976049 0.418941 0.059 Uiso 1 1 calc R U . . .
C28 C 0.3517(3) 0.9010(2) 0.2810(2) 0.0482(14) Uani 1 1 d . . . . .
H28 H 0.350066 0.944993 0.297755 0.058 Uiso 1 1 calc R U . . .
C40 C 0.0487(3) 0.9078(2) 0.6295(3) 0.0558(15) Uani 1 1 d . . . . .
H40A H 0.010536 0.895873 0.592728 0.084 Uiso 1 1 calc R U . . .
H40B H 0.061370 0.956042 0.628898 0.084 Uiso 1 1 calc R U . . .
H40C H 0.020136 0.897094 0.666413 0.084 Uiso 1 1 calc R U . . .
C45 C 0.0265(3) 0.7360(2) 0.4463(2) 0.0435(12) Uani 1 1 d . . . . .
H45A H -0.007867 0.776480 0.436313 0.065 Uiso 1 1 calc R U . . .
H45B H 0.031794 0.728732 0.490933 0.065 Uiso 1 1 calc R U . . .
H45C H -0.001996 0.697174 0.425531 0.065 Uiso 1 1 calc R U . . .
C49 C 0.1642(3) 0.9574(2) 0.4883(2) 0.0516(14) Uani 1 1 d . . . . .
H49A H 0.199327 0.973014 0.456225 0.077 Uiso 1 1 calc R U . . .
H49B H 0.201892 0.946762 0.525700 0.077 Uiso 1 1 calc R U . . .
H49C H 0.123435 0.992749 0.497398 0.077 Uiso 1 1 calc R U . . .
C9 C 0.8468(3) 0.9026(2) 0.0646(2) 0.0533(14) Uani 1 1 d . . . . .
H9A H 0.885893 0.891276 0.101065 0.080 Uiso 1 1 calc R U . . .
H9B H 0.832519 0.950502 0.065328 0.080 Uiso 1 1 calc R U . . .
H9C H 0.874958 0.892505 0.027382 0.080 Uiso 1 1 calc R U . . .
C39 C 0.1901(3) 0.8823(2) 0.6907(2) 0.0509(14) Uani 1 1 d . . . . .
H39A H 0.162048 0.864417 0.725568 0.076 Uiso 1 1 calc R U . . .
H39B H 0.197989 0.930933 0.695730 0.076 Uiso 1 1 calc R U . . .
H39C H 0.246565 0.860791 0.689315 0.076 Uiso 1 1 calc R U . . .
C55 C 0.3439(3) 0.6214(2) 0.3588(2) 0.0485(13) Uani 1 1 d . . . . .
H55 H 0.320067 0.610030 0.318431 0.058 Uiso 1 1 calc R U . . .
C65 C 0.8794(4) 0.5455(2) 0.3719(3) 0.0559(15) Uani 1 1 d . . . . .
H65 H 0.833869 0.554132 0.396831 0.067 Uiso 1 1 calc R U . . .
C64 C 0.8610(4) 0.5231(3) 0.3135(3) 0.0627(17) Uani 1 1 d . . . . .
H64 H 0.802526 0.516026 0.297944 0.075 Uiso 1 1 calc R U . . .
C66 C 0.9625(4) 0.5557(3) 0.3948(3) 0.0624(16) Uani 1 1 d . . . . .
H66 H 0.975095 0.570426 0.436082 0.075 Uiso 1 1 calc R U . . .
C67 C 1.0282(4) 0.5451(3) 0.3589(3) 0.0637(16) Uani 1 1 d . . . . .
H67 H 1.086167 0.553850 0.374801 0.076 Uiso 1 1 calc R U . . .
C68 C 1.0108(4) 0.5217(3) 0.2999(3) 0.0661(17) Uani 1 1 d . . . . .
H68 H 1.056706 0.513217 0.275157 0.079 Uiso 1 1 calc R U . . .
C48 C 0.0681(4) 0.9091(3) 0.4010(3) 0.078(2) Uani 1 1 d . . . . .
H48A H 0.034563 0.950649 0.402514 0.117 Uiso 1 1 calc R U . . .
H48B H 0.029418 0.871972 0.387596 0.117 Uiso 1 1 calc R U . . .
H48C H 0.111673 0.914573 0.371760 0.117 Uiso 1 1 calc R U . . .
C63 C 0.9258(5) 0.5105(3) 0.2764(3) 0.0714(19) Uani 1 1 d . . . . .
H63 H 0.912598 0.494351 0.235614 0.086 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N1 1.924(3) . ?
Ge1 Cl1 2.3554(11) . ?
Ge1 P1 2.4716(12) . ?
Ge2 N2 1.916(3) . ?
Ge2 Cl2 2.3416(12) . ?
Ge2 P2 2.4615(13) . ?
P1 C19 1.807(4) . ?
P1 C20 1.822(4) . ?
P1 C26 1.823(4) . ?
P2 C50 1.804(4) . ?
P2 C51 1.813(4) . ?
P2 C57 1.816(4) . ?
Si1 N1 1.744(3) . ?
Si1 C19 1.898(4) . ?
Si1 C13 1.904(4) . ?
Si1 C16 1.908(4) . ?
Si2 N2 1.744(3) . ?
Si2 C44 1.887(4) . ?
Si2 C47 1.896(4) . ?
Si2 C50 1.901(5) . ?
N1 C1 1.460(5) . ?
N2 C32 1.458(5) . ?
C26 C27 1.393(6) . ?
C26 C31 1.394(6) . ?
C41 C37 1.515(6) . ?
C41 C42 1.541(6) . ?
C41 C43 1.540(6) . ?
C1 C2 1.410(6) . ?
C1 C6 1.414(5) . ?
C6 C5 1.400(6) . ?
C6 C10 1.528(5) . ?
C10 C11 1.528(6) . ?
C10 C12 1.531(6) . ?
C32 C37 1.413(5) . ?
C32 C33 1.423(6) . ?
C20 C25 1.392(6) . ?
C20 C21 1.404(6) . ?
C37 C36 1.398(6) . ?
C57 C58 1.390(6) . ?
C57 C62 1.399(6) . ?
C51 C52 1.386(6) . ?
C51 C56 1.409(6) . ?
C33 C34 1.403(6) . ?
C33 C38 1.513(6) . ?
C36 C35 1.379(6) . ?
C21 C22 1.374(6) . ?
C31 C30 1.383(6) . ?
C13 C14 1.535(6) . ?
C13 C15 1.547(6) . ?
C58 C59 1.398(6) . ?
C25 C24 1.395(6) . ?
C52 C53 1.387(6) . ?
C16 C18 1.536(6) . ?
C16 C17 1.542(6) . ?
C38 C40 1.534(6) . ?
C38 C39 1.540(6) . ?
C2 C3 1.396(6) . ?
C2 C7 1.518(6) . ?
C7 C9 1.531(6) . ?
C7 C8 1.544(6) . ?
C34 C35 1.386(6) . ?
C23 C24 1.377(7) . ?
C23 C22 1.395(6) . ?
C5 C4 1.379(6) . ?
C44 C45 1.540(6) . ?
C44 C46 1.545(6) . ?
C56 C55 1.382(6) . ?
C53 C54 1.374(7) . ?
C54 C55 1.385(7) . ?
C30 C29 1.371(6) . ?
C29 C28 1.379(7) . ?
C60 C61 1.372(7) . ?
C60 C59 1.382(7) . ?
C27 C28 1.377(6) . ?
C47 C48 1.546(7) . ?
C47 C49 1.550(6) . ?
C62 C61 1.390(6) . ?
C4 C3 1.377(6) . ?
C65 C64 1.353(8) . ?
C65 C66 1.355(8) . ?
C64 C63 1.375(8) . ?
C66 C67 1.363(8) . ?
C67 C68 1.371(8) . ?
C68 C63 1.389(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ge1 Cl1 100.69(10) . . ?
N1 Ge1 P1 85.83(10) . . ?
Cl1 Ge1 P1 85.97(4) . . ?
N2 Ge2 Cl2 99.99(10) . . ?
N2 Ge2 P2 86.03(11) . . ?
Cl2 Ge2 P2 87.11(4) . . ?
C19 P1 C20 109.28(19) . . ?
C19 P1 C26 110.42(18) . . ?
C20 P1 C26 107.51(18) . . ?
C19 P1 Ge1 100.45(14) . . ?
C20 P1 Ge1 111.32(13) . . ?
C26 P1 Ge1 117.56(14) . . ?
C50 P2 C51 109.4(2) . . ?
C50 P2 C57 109.7(2) . . ?
C51 P2 C57 106.7(2) . . ?
C50 P2 Ge2 101.31(15) . . ?
C51 P2 Ge2 109.72(13) . . ?
C57 P2 Ge2 119.73(14) . . ?
N1 Si1 C19 102.83(17) . . ?
N1 Si1 C13 111.51(17) . . ?
C19 Si1 C13 110.29(18) . . ?
N1 Si1 C16 114.15(18) . . ?
C19 Si1 C16 106.90(18) . . ?
C13 Si1 C16 110.74(19) . . ?
N2 Si2 C44 110.81(17) . . ?
N2 Si2 C47 115.07(19) . . ?
C44 Si2 C47 110.0(2) . . ?
N2 Si2 C50 102.80(18) . . ?
C44 Si2 C50 110.5(2) . . ?
C47 Si2 C50 107.4(2) . . ?
C1 N1 Si1 123.1(3) . . ?
C1 N1 Ge1 110.4(2) . . ?
Si1 N1 Ge1 126.17(18) . . ?
C32 N2 Si2 121.9(3) . . ?
C32 N2 Ge2 111.3(2) . . ?
Si2 N2 Ge2 126.51(19) . . ?
C27 C26 C31 119.0(4) . . ?
C27 C26 P1 121.6(3) . . ?
C31 C26 P1 119.1(3) . . ?
C37 C41 C42 110.7(3) . . ?
C37 C41 C43 113.4(4) . . ?
C42 C41 C43 109.7(3) . . ?
C2 C1 C6 119.5(4) . . ?
C2 C1 N1 119.9(3) . . ?
C6 C1 N1 120.6(3) . . ?
C5 C6 C1 119.1(4) . . ?
C5 C6 C10 117.9(4) . . ?
C1 C6 C10 123.0(4) . . ?
C11 C10 C6 111.2(3) . . ?
C11 C10 C12 110.3(3) . . ?
C6 C10 C12 111.7(4) . . ?
P1 C19 Si1 110.6(2) . . ?
C37 C32 C33 119.6(4) . . ?
C37 C32 N2 120.8(4) . . ?
C33 C32 N2 119.5(3) . . ?
C25 C20 C21 119.1(4) . . ?
C25 C20 P1 118.7(3) . . ?
C21 C20 P1 122.2(3) . . ?
C36 C37 C32 119.0(4) . . ?
C36 C37 C41 118.0(4) . . ?
C32 C37 C41 122.9(4) . . ?
C58 C57 C62 118.9(4) . . ?
C58 C57 P2 119.8(3) . . ?
C62 C57 P2 121.2(4) . . ?
C52 C51 C56 118.4(4) . . ?
C52 C51 P2 119.2(3) . . ?
C56 C51 P2 122.4(3) . . ?
C34 C33 C32 118.4(4) . . ?
C34 C33 C38 119.1(4) . . ?
C32 C33 C38 122.4(4) . . ?
C35 C36 C37 121.6(4) . . ?
C22 C21 C20 120.1(4) . . ?
C30 C31 C26 120.5(4) . . ?
C14 C13 C15 110.1(3) . . ?
C14 C13 Si1 116.1(3) . . ?
C15 C13 Si1 111.5(3) . . ?
C57 C58 C59 120.1(4) . . ?
C20 C25 C24 120.2(4) . . ?
C51 C52 C53 121.3(4) . . ?
P2 C50 Si2 111.3(2) . . ?
C18 C16 C17 108.6(4) . . ?
C18 C16 Si1 113.0(3) . . ?
C17 C16 Si1 113.4(3) . . ?
C33 C38 C40 113.4(4) . . ?
C33 C38 C39 109.7(4) . . ?
C40 C38 C39 109.5(4) . . ?
C3 C2 C1 118.9(4) . . ?
C3 C2 C7 118.3(4) . . ?
C1 C2 C7 122.8(4) . . ?
C2 C7 C9 114.3(4) . . ?
C2 C7 C8 109.7(4) . . ?
C9 C7 C8 109.9(4) . . ?
C35 C34 C33 121.7(4) . . ?
C24 C23 C22 119.5(4) . . ?
C4 C5 C6 121.1(4) . . ?
C45 C44 C46 109.5(4) . . ?
C45 C44 Si2 112.1(3) . . ?
C46 C44 Si2 117.5(3) . . ?
C23 C24 C25 120.4(4) . . ?
C55 C56 C51 119.8(4) . . ?
C54 C53 C52 119.8(4) . . ?
C53 C54 C55 120.0(4) . . ?
C36 C35 C34 119.3(4) . . ?
C29 C30 C31 120.0(5) . . ?
C30 C29 C28 119.9(4) . . ?
C61 C60 C59 120.6(4) . . ?
C28 C27 C26 119.7(4) . . ?
C48 C47 C49 107.5(4) . . ?
C48 C47 Si2 112.8(3) . . ?
C49 C47 Si2 114.7(3) . . ?
C60 C59 C58 119.9(5) . . ?
C61 C62 C57 120.6(5) . . ?
C3 C4 C5 119.7(4) . . ?
C21 C22 C23 120.8(4) . . ?
C4 C3 C2 121.5(4) . . ?
C60 C61 C62 119.9(5) . . ?
C27 C28 C29 120.9(4) . . ?
C56 C55 C54 120.7(5) . . ?
C64 C65 C66 120.2(6) . . ?
C65 C64 C63 121.0(6) . . ?
C65 C66 C67 120.4(6) . . ?
C66 C67 C68 120.2(6) . . ?
C67 C68 C63 119.6(6) . . ?
C64 C63 C68 118.7(6) . . ?

_refine_diff_density_max         0.403
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.089


####################################################################### 
# 
# 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_compound_5a
_database_code_depnum_ccdc_archive 'CCDC 2057305'
loop_
_audit_author_name
_audit_author_address
'Terrance Hadlington'
;TU Munich
Germany
;
_audit_update_record             
;
2021-01-19 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C73 H71 Ge N2 Ni P3 Si'
_chemical_formula_sum            'C73 H71 Ge N2 Ni P3 Si'
_chemical_formula_weight         1228.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'
Ni Ni 0.3393 1.1124 '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'

_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                   12.180(2)
_cell_length_b                   13.550(3)
_cell_length_c                   20.860(4)
_cell_angle_alpha                75.10(3)
_cell_angle_beta                 88.30(3)
_cell_angle_gamma                70.40(3)
_cell_volume                     3128.1(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2000
_cell_measurement_theta_min      1.92
_cell_measurement_theta_max      32.50

_exptl_crystal_description       block
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    0.922
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'STOE X-AREA 1.76'

_diffrn_ambient_temperature      150(2)
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            32911
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.931
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             12253
_reflns_number_gt                9346
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0518P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12253
_refine_ls_number_parameters     736
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0364
_refine_ls_wR_factor_ref         0.0912
_refine_ls_wR_factor_gt          0.0831
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_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
Ge1 Ge 0.20579(2) 0.43811(2) 0.31554(2) 0.01802(7) Uani 1 1 d . . . . .
Ni1 Ni 0.15253(3) 0.58901(2) 0.23334(2) 0.01620(8) Uani 1 1 d . . . . .
P1 P 0.29785(5) 0.54632(5) 0.16825(3) 0.01701(13) Uani 1 1 d . . . . .
P3 P -0.03025(5) 0.61952(5) 0.20584(3) 0.01798(13) Uani 1 1 d . . . . .
P2 P 0.16005(5) 0.72335(5) 0.27202(3) 0.01835(13) Uani 1 1 d . . . . .
Si1 Si 0.45069(6) 0.31075(5) 0.26926(3) 0.01749(14) Uani 1 1 d . . . . .
N1 N 0.34647(16) 0.31855(15) 0.32928(9) 0.0178(4) Uani 1 1 d . . . . .
N2 N 0.13177(19) 0.38954(17) 0.38752(10) 0.0282(5) Uani 1 1 d . . . . .
C26 C 0.2905(2) 0.48010(19) 0.10165(11) 0.0225(5) Uani 1 1 d . . . . .
C1 C 0.3686(2) 0.24053(18) 0.39369(11) 0.0184(5) Uani 1 1 d . . . . .
C32 C 0.3500(2) 0.65512(18) 0.11761(11) 0.0198(5) Uani 1 1 d . . . . .
C38 C 0.1273(2) 0.7273(2) 0.35922(11) 0.0217(5) Uani 1 1 d . . . . .
C25 C 0.4356(2) 0.45155(18) 0.21627(11) 0.0192(5) Uani 1 1 d . . . . .
H25A H 0.456185 0.489971 0.245958 0.023 Uiso 1 1 calc R U . . .
H25B H 0.496891 0.442137 0.183917 0.023 Uiso 1 1 calc R U . . .
C13 C 0.6034(2) 0.24908(19) 0.31068(11) 0.0200(5) Uani 1 1 d . . . . .
C62 C -0.0798(2) 0.51010(19) 0.19106(11) 0.0209(5) Uani 1 1 d . . . . .
C24 C 0.3396(2) 0.2220(2) 0.18836(12) 0.0257(6) Uani 1 1 d . . . . .
H24 H 0.267946 0.267067 0.200143 0.031 Uiso 1 1 calc R U . . .
C2 C 0.3249(2) 0.15267(19) 0.40614(12) 0.0226(5) Uani 1 1 d . . . . .
C31 C 0.1871(2) 0.4672(2) 0.08565(12) 0.0263(6) Uani 1 1 d . . . . .
H31 H 0.119547 0.493915 0.108558 0.032 Uiso 1 1 calc R U . . .
C10 C 0.4682(2) 0.3544(2) 0.43726(12) 0.0236(5) Uani 1 1 d . . . . .
H10 H 0.467655 0.387380 0.388473 0.028 Uiso 1 1 calc R U . . .
C19 C 0.4456(2) 0.22058(18) 0.21434(11) 0.0207(5) Uani 1 1 d . . . . .
C56 C -0.1242(2) 0.6547(2) 0.27352(12) 0.0233(5) Uani 1 1 d . . . . .
C50 C 0.3066(2) 0.7361(2) 0.27417(12) 0.0227(5) Uani 1 1 d . . . . .
C33 C 0.4451(2) 0.67766(19) 0.13784(12) 0.0231(5) Uani 1 1 d . . . . .
H33 H 0.488860 0.633844 0.178208 0.028 Uiso 1 1 calc R U . . .
C55 C 0.3947(2) 0.6467(2) 0.31281(12) 0.0286(6) Uani 1 1 d . . . . .
H55 H 0.377406 0.583938 0.335822 0.034 Uiso 1 1 calc R U . . .
C73 C -0.0376(2) 0.7353(2) 0.07413(13) 0.0280(6) Uani 1 1 d . . . . .
H73 H 0.040729 0.687408 0.077027 0.034 Uiso 1 1 calc R U . . .
C68 C -0.1029(2) 0.72865(18) 0.13068(12) 0.0206(5) Uani 1 1 d . . . . .
C39 C 0.0690(2) 0.6611(2) 0.39612(12) 0.0265(6) Uani 1 1 d . . . . .
H39 H 0.045951 0.614643 0.376419 0.032 Uiso 1 1 calc R U . . .
C44 C 0.0683(2) 0.86100(19) 0.22397(12) 0.0216(5) Uani 1 1 d . . . . .
C14 C 0.6442(2) 0.1389(2) 0.34670(12) 0.0254(5) Uani 1 1 d . . . . .
H14 H 0.593654 0.097749 0.350456 0.031 Uiso 1 1 calc R U . . .
C20 C 0.5489(2) 0.1535(2) 0.19485(12) 0.0296(6) Uani 1 1 d . . . . .
H20 H 0.621803 0.151671 0.211075 0.035 Uiso 1 1 calc R U . . .
C69 C -0.2180(2) 0.8014(2) 0.12486(13) 0.0261(6) Uani 1 1 d . . . . .
H69 H -0.264742 0.798359 0.162118 0.031 Uiso 1 1 calc R U . . .
C6 C 0.4264(2) 0.25736(19) 0.44590(11) 0.0211(5) Uani 1 1 d . . . . .
C27 C 0.3888(2) 0.4422(2) 0.06603(12) 0.0311(6) Uani 1 1 d . . . . .
H27 H 0.459491 0.452720 0.075083 0.037 Uiso 1 1 calc R U . . .
C18 C 0.6818(2) 0.3066(2) 0.30599(12) 0.0266(6) Uani 1 1 d . . . . .
H18 H 0.657175 0.381171 0.282385 0.032 Uiso 1 1 calc R U . . .
C7 C 0.2636(2) 0.1298(2) 0.35180(13) 0.0270(6) Uani 1 1 d . . . . .
H7 H 0.253927 0.190477 0.310830 0.032 Uiso 1 1 calc R U . . .
C63 C -0.0022(2) 0.4040(2) 0.20145(13) 0.0289(6) Uani 1 1 d . . . . .
H63 H 0.075709 0.386454 0.218114 0.035 Uiso 1 1 calc R U . . .
C57 C -0.1437(2) 0.5715(2) 0.32313(12) 0.0279(6) Uani 1 1 d . . . . .
H57 H -0.123094 0.500810 0.316636 0.033 Uiso 1 1 calc R U . . .
C23 C 0.3378(3) 0.1581(2) 0.14548(13) 0.0314(6) Uani 1 1 d . . . . .
H23 H 0.265242 0.160244 0.128627 0.038 Uiso 1 1 calc R U . . .
C37 C 0.2874(2) 0.7222(2) 0.05751(13) 0.0305(6) Uani 1 1 d . . . . .
H37 H 0.222389 0.708660 0.042401 0.037 Uiso 1 1 calc R U . . .
C45 C -0.0035(2) 0.9423(2) 0.25204(13) 0.0271(6) Uani 1 1 d . . . . .
H45 H -0.002867 0.929900 0.298988 0.033 Uiso 1 1 calc R U . . .
C15 C 0.7568(2) 0.0886(2) 0.37702(12) 0.0296(6) Uani 1 1 d . . . . .
H15 H 0.781521 0.014702 0.401846 0.036 Uiso 1 1 calc R U . . .
C3 C 0.3397(2) 0.0844(2) 0.47037(13) 0.0298(6) Uani 1 1 d . . . . .
H3 H 0.310261 0.025863 0.479157 0.036 Uiso 1 1 calc R U . . .
C21 C 0.5478(3) 0.0894(2) 0.15233(14) 0.0380(7) Uani 1 1 d . . . . .
H21 H 0.619061 0.044167 0.140271 0.046 Uiso 1 1 calc R U . . .
C30 C 0.1806(3) 0.4157(2) 0.03646(13) 0.0357(7) Uani 1 1 d . . . . .
H30 H 0.109181 0.408150 0.025664 0.043 Uiso 1 1 calc R U . . .
C67 C -0.1943(2) 0.5324(2) 0.16816(13) 0.0301(6) Uani 1 1 d . . . . .
H67 H -0.249397 0.603474 0.162104 0.036 Uiso 1 1 calc R U . . .
C4 C 0.3964(2) 0.1000(2) 0.52172(13) 0.0333(6) Uani 1 1 d . . . . .
H4 H 0.405580 0.052766 0.565146 0.040 Uiso 1 1 calc R U . . .
C61 C -0.1588(2) 0.7597(2) 0.28325(13) 0.0282(6) Uani 1 1 d . . . . .
H61 H -0.147564 0.817589 0.249988 0.034 Uiso 1 1 calc R U . . .
C16 C 0.8324(2) 0.1471(2) 0.37071(13) 0.0316(6) Uani 1 1 d . . . . .
H16 H 0.909616 0.112772 0.390490 0.038 Uiso 1 1 calc R U . . .
C64 C -0.0377(3) 0.3231(2) 0.18757(15) 0.0388(7) Uani 1 1 d . . . . .
H64 H 0.015955 0.251213 0.194756 0.047 Uiso 1 1 calc R U . . .
C5 C 0.4397(2) 0.1856(2) 0.50891(12) 0.0275(6) Uani 1 1 d . . . . .
H5 H 0.479349 0.195457 0.544020 0.033 Uiso 1 1 calc R U . . .
C49 C 0.0660(3) 0.8827(2) 0.15491(13) 0.0327(6) Uani 1 1 d . . . . .
H49 H 0.114190 0.828907 0.134951 0.039 Uiso 1 1 calc R U . . .
C72 C -0.0849(3) 0.8105(2) 0.01381(13) 0.0341(6) Uani 1 1 d . . . . .
H72 H -0.039674 0.812347 -0.024094 0.041 Uiso 1 1 calc R U . . .
C34 C 0.4772(2) 0.7639(2) 0.09956(13) 0.0294(6) Uani 1 1 d . . . . .
H34 H 0.542278 0.777894 0.114158 0.035 Uiso 1 1 calc R U . . .
C12 C 0.3836(2) 0.4417(2) 0.46729(13) 0.0309(6) Uani 1 1 d . . . . .
H12A H 0.304402 0.462296 0.447635 0.046 Uiso 1 1 calc R U . . .
H12B H 0.408065 0.505619 0.457811 0.046 Uiso 1 1 calc R U . . .
H12C H 0.384576 0.412550 0.515488 0.046 Uiso 1 1 calc R U . . .
C54 C 0.5080(2) 0.6483(3) 0.31806(14) 0.0364(7) Uani 1 1 d . . . . .
H54 H 0.567268 0.587049 0.344696 0.044 Uiso 1 1 calc R U . . .
C43 C 0.1587(2) 0.7963(2) 0.38913(13) 0.0304(6) Uani 1 1 d . . . . .
H43 H 0.198667 0.841968 0.364815 0.036 Uiso 1 1 calc R U . . .
C70 C -0.2643(2) 0.8780(2) 0.06480(13) 0.0308(6) Uani 1 1 d . . . . .
H70 H -0.341806 0.927535 0.061789 0.037 Uiso 1 1 calc R U . . .
C17 C 0.7954(2) 0.2559(2) 0.33551(13) 0.0323(6) Uani 1 1 d . . . . .
H17 H 0.847243 0.295865 0.331472 0.039 Uiso 1 1 calc R U . . .
C51 C 0.3334(2) 0.8286(2) 0.24058(13) 0.0301(6) Uani 1 1 d . . . . .
H51 H 0.274489 0.890534 0.214344 0.036 Uiso 1 1 calc R U . . .
C58 C -0.1930(2) 0.5908(2) 0.38208(14) 0.0361(7) Uani 1 1 d . . . . .
H58 H -0.204351 0.533193 0.415560 0.043 Uiso 1 1 calc R U . . .
C52 C 0.4483(3) 0.8286(2) 0.24611(15) 0.0377(7) Uani 1 1 d . . . . .
H52 H 0.466840 0.890762 0.223269 0.045 Uiso 1 1 calc R U . . .
C46 C -0.0755(3) 1.0405(2) 0.21184(14) 0.0367(7) Uani 1 1 d . . . . .
H46 H -0.124159 1.094717 0.231317 0.044 Uiso 1 1 calc R U . . .
C60 C -0.2096(2) 0.7786(2) 0.34176(14) 0.0367(7) Uani 1 1 d . . . . .
H60 H -0.233806 0.849785 0.347798 0.044 Uiso 1 1 calc R U . . .
C11 C 0.5932(2) 0.3210(2) 0.46648(14) 0.0344(6) Uani 1 1 d . . . . .
H11A H 0.594333 0.298691 0.515095 0.052 Uiso 1 1 calc R U . . .
H11B H 0.621333 0.382619 0.452670 0.052 Uiso 1 1 calc R U . . .
H11C H 0.643933 0.260253 0.450375 0.052 Uiso 1 1 calc R U . . .
C41 C 0.0750(3) 0.7311(3) 0.49020(14) 0.0407(7) Uani 1 1 d . . . . .
H41 H 0.057156 0.732336 0.534694 0.049 Uiso 1 1 calc R U . . .
C35 C 0.4147(2) 0.8288(2) 0.04072(13) 0.0325(6) Uani 1 1 d . . . . .
H35 H 0.436760 0.887064 0.014755 0.039 Uiso 1 1 calc R U . . .
C22 C 0.4408(3) 0.0922(2) 0.12754(13) 0.0380(7) Uani 1 1 d . . . . .
H22 H 0.439250 0.048913 0.098512 0.046 Uiso 1 1 calc R U . . .
C40 C 0.0442(3) 0.6623(2) 0.46151(13) 0.0368(7) Uani 1 1 d . . . . .
H40 H 0.005951 0.615598 0.486461 0.044 Uiso 1 1 calc R U . . .
C48 C -0.0049(3) 0.9808(2) 0.11477(14) 0.0432(8) Uani 1 1 d . . . . .
H48 H -0.004449 0.994084 0.067791 0.052 Uiso 1 1 calc R U . . .
C71 C -0.1983(2) 0.8828(2) 0.00928(13) 0.0329(6) Uani 1 1 d . . . . .
H71 H -0.230490 0.935125 -0.031468 0.039 Uiso 1 1 calc R U . . .
C65 C -0.1508(3) 0.3478(2) 0.16347(14) 0.0374(7) Uani 1 1 d . . . . .
H65 H -0.174558 0.293216 0.153390 0.045 Uiso 1 1 calc R U . . .
C9 C 0.1414(3) 0.1262(3) 0.36944(15) 0.0410(7) Uani 1 1 d . . . . .
H9A H 0.147677 0.069155 0.410491 0.061 Uiso 1 1 calc R U . . .
H9B H 0.106076 0.110714 0.333239 0.061 Uiso 1 1 calc R U . . .
H9C H 0.092339 0.196494 0.375849 0.061 Uiso 1 1 calc R U . . .
C66 C -0.2289(3) 0.4517(2) 0.15406(14) 0.0366(7) Uani 1 1 d . . . . .
H66 H -0.306906 0.468419 0.137870 0.044 Uiso 1 1 calc R U . . .
C42 C 0.1320(3) 0.7984(3) 0.45404(13) 0.0372(7) Uani 1 1 d . . . . .
H42 H 0.152800 0.846053 0.473733 0.045 Uiso 1 1 calc R U . . .
C29 C 0.2800(3) 0.3758(2) 0.00358(13) 0.0417(8) Uani 1 1 d . . . . .
H29 H 0.277064 0.338742 -0.028951 0.050 Uiso 1 1 calc R U . . .
C36 C 0.3195(3) 0.8082(2) 0.01996(14) 0.0378(7) Uani 1 1 d . . . . .
H36 H 0.275709 0.852973 -0.020206 0.045 Uiso 1 1 calc R U . . .
C28 C 0.3836(3) 0.3898(2) 0.01798(14) 0.0391(7) Uani 1 1 d . . . . .
H28 H 0.450879 0.363273 -0.005187 0.047 Uiso 1 1 calc R U . . .
C8 C 0.3382(3) 0.0240(2) 0.33523(14) 0.0374(7) Uani 1 1 d . . . . .
H8A H 0.415061 0.028070 0.322731 0.056 Uiso 1 1 calc R U . . .
H8B H 0.299414 0.013795 0.298152 0.056 Uiso 1 1 calc R U . . .
H8C H 0.347692 -0.037434 0.374228 0.056 Uiso 1 1 calc R U . . .
C59 C -0.2251(2) 0.6940(3) 0.39153(14) 0.0387(7) Uani 1 1 d . . . . .
H59 H -0.257601 0.707148 0.431749 0.046 Uiso 1 1 calc R U . . .
C53 C 0.5339(3) 0.7395(3) 0.28427(15) 0.0408(7) Uani 1 1 d . . . . .
H53 H 0.611172 0.740398 0.287517 0.049 Uiso 1 1 calc R U . . .
C47 C -0.0762(3) 1.0595(2) 0.14289(14) 0.0456(8) Uani 1 1 d . . . . .
H47 H -0.125647 1.126506 0.115318 0.055 Uiso 1 1 calc R U . . .
H1 H 0.062249 0.428410 0.392573 0.067(11) Uiso 1 1 d R . . . .
H2 H 0.166949 0.336420 0.416773 0.031(8) Uiso 1 1 d R . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N2 1.819(2) . ?
Ge1 N1 1.890(2) . ?
Ge1 Ni1 2.2170(10) . ?
Ni1 P3 2.1892(9) . ?
Ni1 P2 2.2011(8) . ?
Ni1 P1 2.2103(9) . ?
P1 C26 1.856(2) . ?
P1 C25 1.860(3) . ?
P1 C32 1.866(2) . ?
P3 C56 1.848(2) . ?
P3 C68 1.855(3) . ?
P3 C62 1.872(2) . ?
P2 C50 1.853(3) . ?
P2 C44 1.855(3) . ?
P2 C38 1.861(2) . ?
Si1 N1 1.7532(19) . ?
Si1 C19 1.893(2) . ?
Si1 C13 1.893(3) . ?
Si1 C25 1.894(2) . ?
N1 C1 1.447(3) . ?
C26 C31 1.389(4) . ?
C26 C27 1.408(3) . ?
C1 C6 1.420(3) . ?
C1 C2 1.424(3) . ?
C32 C33 1.395(3) . ?
C32 C37 1.409(4) . ?
C38 C39 1.394(3) . ?
C38 C43 1.401(3) . ?
C13 C18 1.409(3) . ?
C13 C14 1.410(3) . ?
C62 C63 1.396(3) . ?
C62 C67 1.396(4) . ?
C24 C23 1.400(3) . ?
C24 C19 1.407(4) . ?
C2 C3 1.396(4) . ?
C2 C7 1.525(4) . ?
C31 C30 1.399(4) . ?
C10 C6 1.530(3) . ?
C10 C11 1.531(4) . ?
C10 C12 1.542(3) . ?
C19 C20 1.403(3) . ?
C56 C57 1.401(4) . ?
C56 C61 1.409(3) . ?
C50 C55 1.395(4) . ?
C50 C51 1.406(3) . ?
C33 C34 1.401(3) . ?
C55 C54 1.395(4) . ?
C73 C72 1.394(4) . ?
C73 C68 1.403(3) . ?
C68 C69 1.405(3) . ?
C39 C40 1.391(3) . ?
C44 C49 1.394(4) . ?
C44 C45 1.406(3) . ?
C14 C15 1.395(4) . ?
C20 C21 1.395(4) . ?
C69 C70 1.395(4) . ?
C6 C5 1.396(3) . ?
C27 C28 1.384(4) . ?
C18 C17 1.400(4) . ?
C7 C9 1.537(4) . ?
C7 C8 1.537(4) . ?
C63 C64 1.401(4) . ?
C57 C58 1.399(3) . ?
C23 C22 1.380(4) . ?
C37 C36 1.393(4) . ?
C45 C46 1.389(4) . ?
C15 C16 1.386(4) . ?
C3 C4 1.389(4) . ?
C21 C22 1.401(4) . ?
C30 C29 1.389(4) . ?
C67 C66 1.394(4) . ?
C4 C5 1.391(4) . ?
C61 C60 1.396(4) . ?
C16 C17 1.390(4) . ?
C64 C65 1.380(4) . ?
C49 C48 1.384(4) . ?
C72 C71 1.388(4) . ?
C34 C35 1.382(4) . ?
C54 C53 1.387(4) . ?
C43 C42 1.388(3) . ?
C70 C71 1.390(4) . ?
C51 C52 1.407(4) . ?
C58 C59 1.384(4) . ?
C52 C53 1.374(4) . ?
C46 C47 1.394(4) . ?
C60 C59 1.397(4) . ?
C41 C40 1.379(4) . ?
C41 C42 1.387(4) . ?
C35 C36 1.386(4) . ?
C48 C47 1.381(4) . ?
C65 C66 1.377(4) . ?
C29 C28 1.389(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
N2 Ge1 N1 99.07(9) . . ?
N2 Ge1 Ni1 132.29(7) . . ?
N1 Ge1 Ni1 128.63(6) . . ?
P3 Ni1 P2 108.12(4) . . ?
P3 Ni1 P1 124.25(3) . . ?
P2 Ni1 P1 109.70(3) . . ?
P3 Ni1 Ge1 105.50(4) . . ?
P2 Ni1 Ge1 108.48(3) . . ?
P1 Ni1 Ge1 99.57(4) . . ?
C26 P1 C25 101.71(11) . . ?
C26 P1 C32 97.53(11) . . ?
C25 P1 C32 100.53(11) . . ?
C26 P1 Ni1 122.12(9) . . ?
C25 P1 Ni1 112.13(8) . . ?
C32 P1 Ni1 119.33(8) . . ?
C56 P3 C68 104.27(11) . . ?
C56 P3 C62 99.46(11) . . ?
C68 P3 C62 98.58(11) . . ?
C56 P3 Ni1 110.66(8) . . ?
C68 P3 Ni1 119.29(8) . . ?
C62 P3 Ni1 121.60(8) . . ?
C50 P2 C44 102.49(12) . . ?
C50 P2 C38 97.24(11) . . ?
C44 P2 C38 102.32(11) . . ?
C50 P2 Ni1 114.78(8) . . ?
C44 P2 Ni1 115.34(8) . . ?
C38 P2 Ni1 121.59(9) . . ?
N1 Si1 C19 114.00(10) . . ?
N1 Si1 C13 110.35(10) . . ?
C19 Si1 C13 104.86(11) . . ?
N1 Si1 C25 110.23(10) . . ?
C19 Si1 C25 109.96(10) . . ?
C13 Si1 C25 107.09(11) . . ?
C1 N1 Si1 121.98(15) . . ?
C1 N1 Ge1 116.91(14) . . ?
Si1 N1 Ge1 120.83(11) . . ?
C31 C26 C27 118.4(2) . . ?
C31 C26 P1 120.53(18) . . ?
C27 C26 P1 121.0(2) . . ?
C6 C1 C2 120.2(2) . . ?
C6 C1 N1 119.2(2) . . ?
C2 C1 N1 120.5(2) . . ?
C33 C32 C37 117.7(2) . . ?
C33 C32 P1 123.25(18) . . ?
C37 C32 P1 118.99(19) . . ?
C39 C38 C43 118.5(2) . . ?
C39 C38 P2 119.72(18) . . ?
C43 C38 P2 121.78(19) . . ?
P1 C25 Si1 122.97(13) . . ?
C18 C13 C14 117.0(2) . . ?
C18 C13 Si1 123.50(19) . . ?
C14 C13 Si1 119.45(19) . . ?
C63 C62 C67 118.1(2) . . ?
C63 C62 P3 120.69(19) . . ?
C67 C62 P3 121.20(19) . . ?
C23 C24 C19 121.2(2) . . ?
C3 C2 C1 118.7(2) . . ?
C3 C2 C7 118.8(2) . . ?
C1 C2 C7 122.4(2) . . ?
C26 C31 C30 121.3(2) . . ?
C6 C10 C11 112.4(2) . . ?
C6 C10 C12 110.8(2) . . ?
C11 C10 C12 110.8(2) . . ?
C20 C19 C24 117.1(2) . . ?
C20 C19 Si1 120.68(19) . . ?
C24 C19 Si1 122.12(18) . . ?
C57 C56 C61 118.5(2) . . ?
C57 C56 P3 119.21(19) . . ?
C61 C56 P3 121.22(19) . . ?
C55 C50 C51 119.0(2) . . ?
C55 C50 P2 116.30(19) . . ?
C51 C50 P2 124.7(2) . . ?
C32 C33 C34 121.0(2) . . ?
C54 C55 C50 120.8(3) . . ?
C72 C73 C68 121.6(2) . . ?
C73 C68 C69 117.8(2) . . ?
C73 C68 P3 116.38(18) . . ?
C69 C68 P3 125.81(18) . . ?
C40 C39 C38 120.7(2) . . ?
C49 C44 C45 118.0(2) . . ?
C49 C44 P2 117.09(19) . . ?
C45 C44 P2 124.82(19) . . ?
C15 C14 C13 121.9(2) . . ?
C21 C20 C19 122.0(3) . . ?
C70 C69 C68 120.5(2) . . ?
C5 C6 C1 118.4(2) . . ?
C5 C6 C10 118.5(2) . . ?
C1 C6 C10 123.0(2) . . ?
C28 C27 C26 120.6(3) . . ?
C17 C18 C13 121.2(2) . . ?
C2 C7 C9 112.7(2) . . ?
C2 C7 C8 111.1(2) . . ?
C9 C7 C8 110.2(2) . . ?
C62 C63 C64 120.7(3) . . ?
C58 C57 C56 121.1(2) . . ?
C22 C23 C24 120.4(3) . . ?
C36 C37 C32 120.9(3) . . ?
C46 C45 C44 120.7(2) . . ?
C16 C15 C14 119.6(2) . . ?
C4 C3 C2 121.5(2) . . ?
C20 C21 C22 119.6(3) . . ?
C29 C30 C31 119.2(3) . . ?
C66 C67 C62 120.8(3) . . ?
C3 C4 C5 119.3(2) . . ?
C60 C61 C56 120.0(3) . . ?
C15 C16 C17 120.1(3) . . ?
C65 C64 C63 120.0(3) . . ?
C4 C5 C6 121.9(2) . . ?
C48 C49 C44 121.4(2) . . ?
C71 C72 C73 119.8(2) . . ?
C35 C34 C33 120.5(3) . . ?
C53 C54 C55 119.8(3) . . ?
C42 C43 C38 120.5(3) . . ?
C71 C70 C69 120.8(2) . . ?
C16 C17 C18 120.1(3) . . ?
C50 C51 C52 119.5(3) . . ?
C59 C58 C57 119.9(3) . . ?
C53 C52 C51 120.6(3) . . ?
C45 C46 C47 119.9(2) . . ?
C61 C60 C59 120.7(3) . . ?
C40 C41 C42 119.9(2) . . ?
C34 C35 C36 119.4(2) . . ?
C23 C22 C21 119.7(2) . . ?
C41 C40 C39 120.2(3) . . ?
C47 C48 C49 120.1(3) . . ?
C72 C71 C70 119.5(3) . . ?
C66 C65 C64 119.9(3) . . ?
C65 C66 C67 120.4(3) . . ?
C41 C42 C43 120.2(3) . . ?
C30 C29 C28 120.4(2) . . ?
C35 C36 C37 120.5(3) . . ?
C27 C28 C29 120.1(3) . . ?
C58 C59 C60 119.8(2) . . ?
C52 C53 C54 120.3(3) . . ?
C48 C47 C46 119.9(3) . . ?

_refine_diff_density_max         0.443
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.066


####################################################################### 
# 
# 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_compound_3b
_database_code_depnum_ccdc_archive 'CCDC 2057301'
loop_
_audit_author_name
_audit_author_address
'Terrance Hadlington'
;TU Munich
Germany
;
_audit_update_record             
;
2021-01-19 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H43 Br Ge N P Si'
_chemical_formula_sum            'C31 H43 Br Ge N P Si'
_chemical_formula_weight         641.22

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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                   11.110(2)
_cell_length_b                   17.260(4)
_cell_length_c                   18.290(4)
_cell_angle_alpha                65.10(3)
_cell_angle_beta                 88.40(3)
_cell_angle_gamma                85.30(3)
_cell_volume                     3170.5(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2000
_cell_measurement_theta_min      1.92
_cell_measurement_theta_max      32.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    2.334
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.545
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'STOE X-AREA 1.76'

_diffrn_ambient_temperature      150(2)
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            44725
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.955
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             12450
_reflns_number_gt                9873
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1037P)²+17.5730P] 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         12450
_refine_ls_number_parameters     665
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0609
_refine_ls_wR_factor_ref         0.1968
_refine_ls_wR_factor_gt          0.1787
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_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
Ge1 Ge 0.52861(5) -0.03152(3) 0.91532(3) 0.01942(15) Uani 1 1 d . . . . .
Ge2 Ge 0.02771(5) 0.56324(4) 0.56281(3) 0.02108(15) Uani 1 1 d . . . . .
Br1 Br 0.70306(6) 0.05673(5) 0.88375(5) 0.0451(2) Uani 1 1 d . . . . .
Br2 Br 0.21389(6) 0.62222(5) 0.49110(5) 0.0498(2) Uani 1 1 d . . . . .
P1 P 0.41602(11) 0.09766(8) 0.81893(8) 0.0185(3) Uani 1 1 d . . . . .
P2 P 0.15634(12) 0.43617(9) 0.65044(8) 0.0211(3) Uani 1 1 d . . . . .
Si1 Si 0.50986(13) -0.00598(10) 0.72771(9) 0.0208(3) Uani 1 1 d . . . . .
Si2 Si 0.13883(13) 0.56497(10) 0.72565(9) 0.0236(3) Uani 1 1 d . . . . .
N1 N 0.5356(4) -0.0698(3) 0.8302(3) 0.0197(9) Uani 1 1 d . . . . .
N2 N 0.0284(4) 0.5983(3) 0.6497(3) 0.0209(9) Uani 1 1 d . . . . .
C20 C 0.4276(4) 0.1968(3) 0.8297(3) 0.0206(10) Uani 1 1 d . . . . .
C1 C 0.5548(5) -0.1619(3) 0.8618(3) 0.0211(10) Uani 1 1 d . . . . .
C26 C 0.2567(4) 0.0793(3) 0.8215(3) 0.0199(10) Uani 1 1 d . . . . .
C21 C 0.3726(5) 0.2053(4) 0.8951(3) 0.0251(11) Uani 1 1 d . . . . .
H21 H 0.322615 0.162546 0.929196 0.030 Uiso 1 1 calc R U . . .
C19 C 0.4769(5) 0.1060(3) 0.7240(3) 0.0232(11) Uani 1 1 d . . . . .
H19A H 0.552164 0.135867 0.712706 0.028 Uiso 1 1 calc R U . . .
H19B H 0.418221 0.139727 0.680154 0.028 Uiso 1 1 calc R U . . .
C32 C -0.0789(5) 0.6531(3) 0.6476(3) 0.0214(10) Uani 1 1 d . . . . .
C56 C 0.2237(5) 0.3241(4) 0.5811(3) 0.0277(12) Uani 1 1 d . . . . .
H56 H 0.143374 0.307584 0.592673 0.033 Uiso 1 1 calc R U . . .
C57 C 0.0625(5) 0.3553(3) 0.7186(3) 0.0235(11) Uani 1 1 d . . . . .
C6 C 0.6744(5) -0.2016(4) 0.8656(3) 0.0249(11) Uani 1 1 d . . . . .
C38 C -0.2043(5) 0.5206(4) 0.7132(3) 0.0268(12) Uani 1 1 d . . . . .
H38 H -0.122575 0.490345 0.716498 0.032 Uiso 1 1 calc R U . . .
C2 C 0.4566(5) -0.2145(3) 0.8932(3) 0.0230(11) Uani 1 1 d . . . . .
C27 C 0.2081(5) 0.0249(4) 0.8945(4) 0.0261(11) Uani 1 1 d . . . . .
H27 H 0.256910 0.000621 0.941776 0.031 Uiso 1 1 calc R U . . .
C33 C -0.1887(5) 0.6161(4) 0.6806(3) 0.0255(11) Uani 1 1 d . . . . .
C51 C 0.2626(5) 0.3835(3) 0.6051(3) 0.0239(11) Uani 1 1 d . . . . .
C50 C 0.2365(5) 0.4782(4) 0.7082(4) 0.0257(11) Uani 1 1 d . . . . .
H50A H 0.310598 0.502503 0.679128 0.031 Uiso 1 1 calc R U . . .
H50B H 0.261007 0.431188 0.760779 0.031 Uiso 1 1 calc R U . . .
C13 C 0.6479(5) -0.0028(4) 0.6630(3) 0.0294(12) Uani 1 1 d . . . . .
H13 H 0.682247 -0.063279 0.680379 0.035 Uiso 1 1 calc R U . . .
C37 C -0.0769(5) 0.7431(4) 0.6100(3) 0.0258(11) Uani 1 1 d . . . . .
C16 C 0.3751(5) -0.0393(4) 0.6893(4) 0.0271(12) Uani 1 1 d . . . . .
H16 H 0.313543 -0.052881 0.733031 0.033 Uiso 1 1 calc R U . . .
C3 C 0.4783(5) -0.3029(4) 0.9201(4) 0.0309(13) Uani 1 1 d . . . . .
H3 H 0.412976 -0.338164 0.940799 0.037 Uiso 1 1 calc R U . . .
C7 C 0.3292(5) -0.1789(4) 0.9022(3) 0.0251(11) Uani 1 1 d . . . . .
H7 H 0.326432 -0.115020 0.872978 0.030 Uiso 1 1 calc R U . . .
C31 C 0.1839(5) 0.1145(4) 0.7526(4) 0.0284(12) Uani 1 1 d . . . . .
H31 H 0.215973 0.152267 0.702827 0.034 Uiso 1 1 calc R U . . .
C10 C 0.7857(5) -0.1522(4) 0.8489(3) 0.0254(11) Uani 1 1 d . . . . .
H10 H 0.758508 -0.089817 0.823112 0.030 Uiso 1 1 calc R U . . .
C22 C 0.3892(5) 0.2748(4) 0.9117(4) 0.0278(12) Uani 1 1 d . . . . .
H22 H 0.351100 0.279774 0.956860 0.033 Uiso 1 1 calc R U . . .
C62 C -0.0455(5) 0.3428(4) 0.6889(4) 0.0278(12) Uani 1 1 d . . . . .
H62 H -0.066392 0.375144 0.633645 0.033 Uiso 1 1 calc R U . . .
C39 C -0.2814(5) 0.5034(4) 0.6541(4) 0.0328(13) Uani 1 1 d . . . . .
H39A H -0.362846 0.531202 0.650905 0.049 Uiso 1 1 calc R U . . .
H39B H -0.286177 0.441524 0.673010 0.049 Uiso 1 1 calc R U . . .
H39C H -0.244452 0.526490 0.600604 0.049 Uiso 1 1 calc R U . . .
C28 C 0.0885(5) 0.0060(4) 0.8981(4) 0.0321(13) Uani 1 1 d . . . . .
H28 H 0.054774 -0.030192 0.947984 0.039 Uiso 1 1 calc R U . . .
C4 C 0.5919(6) -0.3409(4) 0.9175(4) 0.0334(13) Uani 1 1 d . . . . .
H4 H 0.603279 -0.400888 0.932960 0.040 Uiso 1 1 calc R U . . .
C9 C 0.3025(5) -0.2008(4) 0.9907(4) 0.0342(13) Uani 1 1 d . . . . .
H9A H 0.223452 -0.173609 0.995259 0.051 Uiso 1 1 calc R U . . .
H9B H 0.364961 -0.179906 1.013124 0.051 Uiso 1 1 calc R U . . .
H9C H 0.302037 -0.263104 1.020727 0.051 Uiso 1 1 calc R U . . .
C55 C 0.3001(6) 0.2874(4) 0.5401(4) 0.0347(14) Uani 1 1 d . . . . .
H55 H 0.272082 0.246642 0.523514 0.042 Uiso 1 1 calc R U . . .
C11 C 0.8497(5) -0.1702(4) 0.9288(4) 0.0310(13) Uani 1 1 d . . . . .
H11A H 0.794017 -0.153815 0.963278 0.046 Uiso 1 1 calc R U . . .
H11B H 0.920690 -0.136870 0.917564 0.046 Uiso 1 1 calc R U . . .
H11C H 0.875230 -0.231405 0.956395 0.046 Uiso 1 1 calc R U . . .
C36 C -0.1820(5) 0.7944(4) 0.6089(4) 0.0297(12) Uani 1 1 d . . . . .
H36 H -0.180662 0.854941 0.583404 0.036 Uiso 1 1 calc R U . . .
C41 C 0.0327(5) 0.7858(4) 0.5651(4) 0.0314(13) Uani 1 1 d . . . . .
H41 H 0.102089 0.741189 0.580546 0.038 Uiso 1 1 calc R U . . .
C14 C 0.7476(5) 0.0471(4) 0.6759(4) 0.0356(14) Uani 1 1 d . . . . .
H14A H 0.826048 0.026762 0.662015 0.053 Uiso 1 1 calc R U . . .
H14B H 0.748774 0.038072 0.732527 0.053 Uiso 1 1 calc R U . . .
H14C H 0.731563 0.108369 0.641458 0.053 Uiso 1 1 calc R U . . .
C29 C 0.0182(5) 0.0403(4) 0.8283(4) 0.0375(15) Uani 1 1 d . . . . .
H29 H -0.063020 0.026087 0.830317 0.045 Uiso 1 1 calc R U . . .
C47 C 0.0625(6) 0.5198(4) 0.8278(4) 0.0335(13) Uani 1 1 d . . . . .
H47 H -0.005340 0.488531 0.821362 0.040 Uiso 1 1 calc R U . . .
C5 C 0.6885(5) -0.2906(4) 0.8923(4) 0.0314(13) Uani 1 1 d . . . . .
H5 H 0.766984 -0.317347 0.893001 0.038 Uiso 1 1 calc R U . . .
C17 C 0.4028(6) -0.1226(4) 0.6781(4) 0.0345(14) Uani 1 1 d . . . . .
H17A H 0.327128 -0.143578 0.670203 0.052 Uiso 1 1 calc R U . . .
H17B H 0.444669 -0.165981 0.726163 0.052 Uiso 1 1 calc R U . . .
H17C H 0.454338 -0.111209 0.630883 0.052 Uiso 1 1 calc R U . . .
C58 C 0.0908(6) 0.3072(4) 0.7996(4) 0.0370(14) Uani 1 1 d . . . . .
H58 H 0.164291 0.314227 0.820675 0.044 Uiso 1 1 calc R U . . .
C54 C 0.4172(6) 0.3115(4) 0.5240(4) 0.0406(16) Uani 1 1 d . . . . .
H54 H 0.470092 0.286863 0.496554 0.049 Uiso 1 1 calc R U . . .
C25 C 0.4992(6) 0.2608(4) 0.7789(4) 0.0333(13) Uani 1 1 d . . . . .
H25 H 0.536496 0.256516 0.733283 0.040 Uiso 1 1 calc R U . . .
C52 C 0.3814(5) 0.4080(4) 0.5870(4) 0.0354(14) Uani 1 1 d . . . . .
H52 H 0.409079 0.450083 0.601869 0.042 Uiso 1 1 calc R U . . .
C40 C -0.2595(6) 0.4839(4) 0.7974(4) 0.0407(15) Uani 1 1 d . . . . .
H40A H -0.216261 0.502246 0.832646 0.061 Uiso 1 1 calc R U . . .
H40B H -0.252648 0.421172 0.819493 0.061 Uiso 1 1 calc R U . . .
H40C H -0.344797 0.504652 0.794056 0.061 Uiso 1 1 calc R U . . .
C23 C 0.4622(5) 0.3374(4) 0.8617(4) 0.0311(13) Uani 1 1 d . . . . .
H23 H 0.475423 0.384908 0.872956 0.037 Uiso 1 1 calc R U . . .
C34 C -0.2906(5) 0.6707(4) 0.6792(4) 0.0340(14) Uani 1 1 d . . . . .
H34 H -0.363440 0.646456 0.703079 0.041 Uiso 1 1 calc R U . . .
C44 C 0.2482(5) 0.6475(4) 0.7203(4) 0.0339(14) Uani 1 1 d . . . . .
H44 H 0.198911 0.699176 0.718928 0.041 Uiso 1 1 calc R U . . .
C35 C -0.2876(5) 0.7587(4) 0.6440(4) 0.0342(14) Uani 1 1 d . . . . .
H35 H -0.357360 0.794414 0.643945 0.041 Uiso 1 1 calc R U . . .
C48 C 0.0026(7) 0.5899(5) 0.8504(4) 0.0450(17) Uani 1 1 d . . . . .
H48A H -0.049852 0.564056 0.897009 0.068 Uiso 1 1 calc R U . . .
H48B H -0.045653 0.631720 0.804693 0.068 Uiso 1 1 calc R U . . .
H48C H 0.065028 0.618799 0.863913 0.068 Uiso 1 1 calc R U . . .
C53 C 0.4579(6) 0.3711(5) 0.5476(4) 0.0425(16) Uani 1 1 d . . . . .
H53 H 0.538636 0.386794 0.536740 0.051 Uiso 1 1 calc R U . . .
C30 C 0.0657(5) 0.0947(4) 0.7565(4) 0.0365(14) Uani 1 1 d . . . . .
H30 H 0.016743 0.118667 0.709219 0.044 Uiso 1 1 calc R U . . .
C61 C -0.1219(6) 0.2841(4) 0.7388(5) 0.0392(15) Uani 1 1 d . . . . .
H61 H -0.194120 0.275191 0.717866 0.047 Uiso 1 1 calc R U . . .
C12 C 0.8765(6) -0.1700(5) 0.7921(4) 0.0384(15) Uani 1 1 d . . . . .
H12A H 0.917665 -0.227143 0.820310 0.058 Uiso 1 1 calc R U . . .
H12B H 0.936035 -0.126956 0.774799 0.058 Uiso 1 1 calc R U . . .
H12C H 0.833681 -0.167142 0.744762 0.058 Uiso 1 1 calc R U . . .
C8 C 0.2312(5) -0.2092(4) 0.8667(4) 0.0372(14) Uani 1 1 d . . . . .
H8A H 0.251488 -0.198520 0.810977 0.056 Uiso 1 1 calc R U . . .
H8B H 0.153843 -0.177874 0.867600 0.056 Uiso 1 1 calc R U . . .
H8C H 0.224844 -0.270646 0.898636 0.056 Uiso 1 1 calc R U . . .
C43 C 0.0680(7) 0.8582(5) 0.5866(5) 0.0516(19) Uani 1 1 d . . . . .
H43A H 0.002969 0.904244 0.570049 0.077 Uiso 1 1 calc R U . . .
H43B H 0.142441 0.880741 0.558503 0.077 Uiso 1 1 calc R U . . .
H43C H 0.080995 0.835675 0.644927 0.077 Uiso 1 1 calc R U . . .
C24 C 0.5153(6) 0.3302(4) 0.7954(4) 0.0384(15) Uani 1 1 d . . . . .
H24 H 0.563721 0.373687 0.760703 0.046 Uiso 1 1 calc R U . . .
C18 C 0.3120(6) 0.0297(4) 0.6132(4) 0.0373(14) Uani 1 1 d . . . . .
H18A H 0.365725 0.041853 0.566858 0.056 Uiso 1 1 calc R U . . .
H18B H 0.292848 0.082148 0.620963 0.056 Uiso 1 1 calc R U . . .
H18C H 0.237315 0.009037 0.603248 0.056 Uiso 1 1 calc R U . . .
C42 C 0.0127(6) 0.8188(5) 0.4740(4) 0.0444(17) Uani 1 1 d . . . . .
H42A H -0.010228 0.771907 0.461740 0.067 Uiso 1 1 calc R U . . .
H42B H 0.087390 0.840415 0.445736 0.067 Uiso 1 1 calc R U . . .
H42C H -0.051935 0.865123 0.456411 0.067 Uiso 1 1 calc R U . . .
C60 C -0.0925(8) 0.2378(4) 0.8204(4) 0.0469(18) Uani 1 1 d . . . . .
H60 H -0.145842 0.198362 0.855473 0.056 Uiso 1 1 calc R U . . .
C46 C 0.3306(6) 0.6768(5) 0.6466(4) 0.0405(15) Uani 1 1 d . . . . .
H46A H 0.374370 0.724684 0.644533 0.061 Uiso 1 1 calc R U . . .
H46B H 0.281703 0.695225 0.597524 0.061 Uiso 1 1 calc R U . . .
H46C H 0.388535 0.629154 0.650556 0.061 Uiso 1 1 calc R U . . .
C49 C 0.1380(7) 0.4534(5) 0.9002(4) 0.0449(17) Uani 1 1 d . . . . .
H49A H 0.197745 0.482470 0.915834 0.067 Uiso 1 1 calc R U . . .
H49B H 0.179453 0.410206 0.884856 0.067 Uiso 1 1 calc R U . . .
H49C H 0.084402 0.425571 0.945704 0.067 Uiso 1 1 calc R U . . .
C45 C 0.3293(7) 0.6120(5) 0.7968(5) 0.0497(19) Uani 1 1 d . . . . .
H45A H 0.370239 0.556787 0.803792 0.075 Uiso 1 1 calc R U . . .
H45B H 0.279219 0.604167 0.843987 0.075 Uiso 1 1 calc R U . . .
H45C H 0.389563 0.652548 0.790921 0.075 Uiso 1 1 calc R U . . .
C15 C 0.6200(7) 0.0327(6) 0.5719(4) 0.054(2) Uani 1 1 d . . . . .
H15A H 0.584089 0.091743 0.552647 0.081 Uiso 1 1 calc R U . . .
H15B H 0.563314 -0.002844 0.562589 0.081 Uiso 1 1 calc R U . . .
H15C H 0.695025 0.031768 0.542684 0.081 Uiso 1 1 calc R U . . .
C59 C 0.0133(8) 0.2495(4) 0.8497(4) 0.0475(18) Uani 1 1 d . . . . .
H59 H 0.033550 0.217557 0.905061 0.057 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N1 1.927(4) . ?
Ge1 P1 2.4496(18) . ?
Ge1 Br1 2.4680(12) . ?
Ge2 N2 1.925(4) . ?
Ge2 P2 2.4648(18) . ?
Ge2 Br2 2.4707(12) . ?
P1 C19 1.798(5) . ?
P1 C20 1.818(5) . ?
P1 C26 1.820(5) . ?
P2 C50 1.799(6) . ?
P2 C57 1.815(6) . ?
P2 C51 1.821(5) . ?
Si1 N1 1.747(5) . ?
Si1 C16 1.899(6) . ?
Si1 C13 1.901(6) . ?
Si1 C19 1.910(6) . ?
Si2 N2 1.753(5) . ?
Si2 C47 1.900(6) . ?
Si2 C50 1.908(5) . ?
Si2 C44 1.916(6) . ?
N1 C1 1.445(7) . ?
N2 C32 1.450(6) . ?
C20 C21 1.384(8) . ?
C20 C25 1.398(8) . ?
C1 C2 1.425(8) . ?
C1 C6 1.434(7) . ?
C26 C31 1.394(8) . ?
C26 C27 1.394(8) . ?
C21 C22 1.383(8) . ?
C32 C37 1.411(8) . ?
C32 C33 1.423(7) . ?
C56 C51 1.375(8) . ?
C56 C55 1.401(8) . ?
C57 C58 1.389(8) . ?
C57 C62 1.400(8) . ?
C6 C5 1.399(8) . ?
C6 C10 1.510(8) . ?
C38 C33 1.521(8) . ?
C38 C40 1.529(8) . ?
C38 C39 1.535(9) . ?
C2 C3 1.395(8) . ?
C2 C7 1.529(7) . ?
C27 C28 1.387(8) . ?
C33 C34 1.406(8) . ?
C51 C52 1.407(8) . ?
C13 C14 1.539(9) . ?
C13 C15 1.544(9) . ?
C37 C36 1.401(8) . ?
C37 C41 1.511(8) . ?
C16 C18 1.540(8) . ?
C16 C17 1.541(8) . ?
C3 C4 1.382(9) . ?
C7 C8 1.517(8) . ?
C7 C9 1.526(8) . ?
C31 C30 1.376(8) . ?
C10 C12 1.533(7) . ?
C10 C11 1.543(8) . ?
C22 C23 1.389(9) . ?
C62 C61 1.378(9) . ?
C28 C29 1.390(9) . ?
C4 C5 1.381(9) . ?
C55 C54 1.384(10) . ?
C36 C35 1.382(9) . ?
C41 C42 1.532(9) . ?
C41 C43 1.540(9) . ?
C29 C30 1.375(10) . ?
C47 C48 1.533(8) . ?
C47 C49 1.548(9) . ?
C58 C59 1.379(10) . ?
C54 C53 1.382(11) . ?
C25 C24 1.377(9) . ?
C52 C53 1.382(9) . ?
C23 C24 1.381(9) . ?
C34 C35 1.381(9) . ?
C44 C46 1.530(10) . ?
C44 C45 1.550(9) . ?
C61 C60 1.397(10) . ?
C60 C59 1.370(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ge1 P1 85.92(13) . . ?
N1 Ge1 Br1 101.83(13) . . ?
P1 Ge1 Br1 85.83(5) . . ?
N2 Ge2 P2 86.33(13) . . ?
N2 Ge2 Br2 101.05(14) . . ?
P2 Ge2 Br2 87.11(5) . . ?
C19 P1 C20 110.7(3) . . ?
C19 P1 C26 108.6(2) . . ?
C20 P1 C26 107.8(2) . . ?
C19 P1 Ge1 102.26(18) . . ?
C20 P1 Ge1 117.49(17) . . ?
C26 P1 Ge1 109.66(18) . . ?
C50 P2 C57 108.4(3) . . ?
C50 P2 C51 110.1(3) . . ?
C57 P2 C51 107.2(2) . . ?
C50 P2 Ge2 101.63(19) . . ?
C57 P2 Ge2 109.65(18) . . ?
C51 P2 Ge2 119.45(18) . . ?
N1 Si1 C16 111.3(2) . . ?
N1 Si1 C13 113.4(2) . . ?
C16 Si1 C13 110.9(3) . . ?
N1 Si1 C19 102.9(2) . . ?
C16 Si1 C19 110.7(2) . . ?
C13 Si1 C19 107.4(3) . . ?
N2 Si2 C47 109.1(3) . . ?
N2 Si2 C50 103.5(2) . . ?
C47 Si2 C50 111.4(3) . . ?
N2 Si2 C44 116.9(3) . . ?
C47 Si2 C44 110.6(3) . . ?
C50 Si2 C44 105.0(3) . . ?
C1 N1 Si1 121.8(3) . . ?
C1 N1 Ge1 111.5(3) . . ?
Si1 N1 Ge1 126.5(2) . . ?
C32 N2 Si2 123.3(4) . . ?
C32 N2 Ge2 111.3(3) . . ?
Si2 N2 Ge2 125.3(2) . . ?
C21 C20 C25 119.0(5) . . ?
C21 C20 P1 118.5(4) . . ?
C25 C20 P1 122.2(4) . . ?
C2 C1 C6 119.3(5) . . ?
C2 C1 N1 120.6(4) . . ?
C6 C1 N1 120.0(5) . . ?
C31 C26 C27 119.3(5) . . ?
C31 C26 P1 122.3(4) . . ?
C27 C26 P1 118.4(4) . . ?
C22 C21 C20 121.2(5) . . ?
P1 C19 Si1 109.6(3) . . ?
C37 C32 C33 119.5(5) . . ?
C37 C32 N2 120.6(5) . . ?
C33 C32 N2 119.8(5) . . ?
C51 C56 C55 121.4(6) . . ?
C58 C57 C62 118.5(5) . . ?
C58 C57 P2 123.0(5) . . ?
C62 C57 P2 118.4(4) . . ?
C5 C6 C1 118.3(5) . . ?
C5 C6 C10 119.0(5) . . ?
C1 C6 C10 122.5(5) . . ?
C33 C38 C40 113.2(5) . . ?
C33 C38 C39 109.5(5) . . ?
C40 C38 C39 110.3(5) . . ?
C3 C2 C1 118.7(5) . . ?
C3 C2 C7 118.1(5) . . ?
C1 C2 C7 123.1(5) . . ?
C28 C27 C26 120.1(5) . . ?
C34 C33 C32 118.6(5) . . ?
C34 C33 C38 117.8(5) . . ?
C32 C33 C38 123.5(5) . . ?
C56 C51 C52 118.9(5) . . ?
C56 C51 P2 119.7(4) . . ?
C52 C51 P2 121.2(5) . . ?
P2 C50 Si2 111.2(3) . . ?
C14 C13 C15 109.0(5) . . ?
C14 C13 Si1 112.7(4) . . ?
C15 C13 Si1 114.2(4) . . ?
C36 C37 C32 119.3(5) . . ?
C36 C37 C41 118.8(5) . . ?
C32 C37 C41 121.7(5) . . ?
C18 C16 C17 109.7(5) . . ?
C18 C16 Si1 116.1(4) . . ?
C17 C16 Si1 113.1(4) . . ?
C4 C3 C2 122.0(6) . . ?
C8 C7 C9 109.7(5) . . ?
C8 C7 C2 113.8(5) . . ?
C9 C7 C2 110.3(5) . . ?
C30 C31 C26 120.3(6) . . ?
C6 C10 C12 114.6(5) . . ?
C6 C10 C11 110.0(5) . . ?
C12 C10 C11 109.3(5) . . ?
C21 C22 C23 119.3(5) . . ?
C61 C62 C57 120.7(6) . . ?
C27 C28 C29 119.7(6) . . ?
C5 C4 C3 119.3(5) . . ?
C54 C55 C56 118.8(6) . . ?
C35 C36 C37 121.4(5) . . ?
C37 C41 C42 110.1(5) . . ?
C37 C41 C43 113.2(6) . . ?
C42 C41 C43 110.8(6) . . ?
C30 C29 C28 120.3(6) . . ?
C48 C47 C49 109.5(5) . . ?
C48 C47 Si2 112.7(5) . . ?
C49 C47 Si2 117.5(5) . . ?
C4 C5 C6 122.0(5) . . ?
C59 C58 C57 120.6(6) . . ?
C53 C54 C55 120.7(6) . . ?
C24 C25 C20 119.6(6) . . ?
C53 C52 C51 120.1(6) . . ?
C24 C23 C22 119.8(5) . . ?
C35 C34 C33 121.7(5) . . ?
C46 C44 C45 108.0(6) . . ?
C46 C44 Si2 115.1(4) . . ?
C45 C44 Si2 110.5(5) . . ?
C34 C35 C36 119.4(5) . . ?
C54 C53 C52 120.2(6) . . ?
C31 C30 C29 120.3(6) . . ?
C62 C61 C60 119.7(6) . . ?
C25 C24 C23 121.0(6) . . ?
C59 C60 C61 119.7(6) . . ?
C60 C59 C58 120.7(6) . . ?

_refine_diff_density_max         1.497
_refine_diff_density_min         -2.283
_refine_diff_density_rms         0.149


####################################################################### 
# 
# 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_compound_4-Br
_database_code_depnum_ccdc_archive 'CCDC 2057304'
loop_
_audit_author_name
_audit_author_address
'Terrance Hadlington'
;TU Munich
Germany
;
_audit_update_record             
;
2021-01-19 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C73 H69 Br Ge N Ni P3 Si'
_chemical_formula_sum            'C73 H69 Br Ge N Ni P3 Si'
_chemical_formula_weight         1292.50

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'
Ni Ni 0.3393 1.1124 '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'
Br Br -0.2901 2.4595 '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                   12.680(3)
_cell_length_b                   15.530(3)
_cell_length_c                   19.470(4)
_cell_angle_alpha                98.60(3)
_cell_angle_beta                 92.00(3)
_cell_angle_gamma                91.30(3)
_cell_volume                     3787.1(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2000
_cell_measurement_theta_min      1.92
_cell_measurement_theta_max      32.5

_exptl_crystal_description       block
_exptl_crystal_colour            purple-brown
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    1.288
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.763
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'STOE X-AREA 1.76'

_diffrn_ambient_temperature      150(2)
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            56477
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.663
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             15676
_reflns_number_gt                11572
_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.
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.528 895 137 'C26 H44'
_platon_squeeze_details          
;
The unit cell contains two hexane molecules and two toluene molecules (one each per asymmetric unit) which have been treated
as a diffuse contribution to the overall scattering without specific atom
positions by SQUEEZE/PLATON.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1019P)²+1.2355P] 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         15676
_refine_ls_number_parameters     734
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0531
_refine_ls_wR_factor_ref         0.1658
_refine_ls_wR_factor_gt          0.1551
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_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
Ge1 Ge 0.69178(3) 0.01716(2) 0.21758(2) 0.01801(11) Uani 1 1 d . . . . .
Ni1 Ni 0.71474(3) -0.12378(3) 0.21073(2) 0.01669(12) Uani 1 1 d . . . . .
Br1 Br 0.55391(4) 0.09018(3) 0.16586(3) 0.04402(14) Uani 1 1 d . . . . .
P1 P 0.83030(7) -0.11779(6) 0.29892(5) 0.0188(2) Uani 1 1 d . . . . .
Si1 Si 0.86236(8) 0.09667(6) 0.33095(5) 0.0191(2) Uani 1 1 d . . . . .
P3 P 0.55249(7) -0.17907(6) 0.21271(5) 0.0191(2) Uani 1 1 d . . . . .
P2 P 0.78833(7) -0.18389(6) 0.11506(5) 0.0186(2) Uani 1 1 d . . . . .
N1 N 0.7609(2) 0.11409(19) 0.27086(15) 0.0194(6) Uani 1 1 d . . . . .
C25 C 0.9144(3) -0.0169(2) 0.30923(19) 0.0199(7) Uani 1 1 d . . . . .
H25A H 0.951743 -0.018103 0.265295 0.024 Uiso 1 1 calc R U . . .
H25B H 0.969011 -0.022931 0.345674 0.024 Uiso 1 1 calc R U . . .
C10 C 0.8799(3) 0.1768(3) 0.1605(2) 0.0269(8) Uani 1 1 d . . . . .
H10 H 0.899893 0.127778 0.185782 0.032 Uiso 1 1 calc R U . . .
C1 C 0.7456(3) 0.2029(2) 0.25801(19) 0.0221(8) Uani 1 1 d . . . . .
C68 C 0.4541(3) -0.1029(2) 0.25323(19) 0.0200(7) Uani 1 1 d . . . . .
C38 C 0.9314(3) -0.1623(2) 0.10689(18) 0.0224(8) Uani 1 1 d . . . . .
C44 C 0.7469(3) -0.1567(2) 0.02864(19) 0.0208(7) Uani 1 1 d . . . . .
C50 C 0.7719(3) -0.3038(2) 0.10247(19) 0.0220(8) Uani 1 1 d . . . . .
C32 C 0.7901(3) -0.1261(2) 0.38865(19) 0.0224(8) Uani 1 1 d . . . . .
C51 C 0.8367(3) -0.3534(2) 0.1413(2) 0.0253(8) Uani 1 1 d . . . . .
H51 H 0.894421 -0.325929 0.169319 0.030 Uiso 1 1 calc R U . . .
C14 C 0.7213(3) 0.0784(3) 0.4405(2) 0.0281(9) Uani 1 1 d . . . . .
H14 H 0.678128 0.045436 0.404662 0.034 Uiso 1 1 calc R U . . .
C56 C 0.4837(3) -0.2198(2) 0.12843(19) 0.0221(8) Uani 1 1 d . . . . .
C13 C 0.8170(3) 0.1151(3) 0.4232(2) 0.0249(8) Uani 1 1 d . . . . .
C62 C 0.5332(3) -0.2719(2) 0.2614(2) 0.0257(8) Uani 1 1 d . . . . .
C33 C 0.8606(3) -0.1075(3) 0.4462(2) 0.0294(9) Uani 1 1 d . . . . .
H33 H 0.929102 -0.084044 0.440668 0.035 Uiso 1 1 calc R U . . .
C24 C 1.0761(3) 0.1458(3) 0.3007(2) 0.0280(9) Uani 1 1 d . . . . .
H24 H 1.084951 0.085461 0.285535 0.034 Uiso 1 1 calc R U . . .
C45 C 0.6946(3) -0.0805(3) 0.0235(2) 0.0260(8) Uani 1 1 d . . . . .
H45 H 0.674849 -0.044279 0.064540 0.031 Uiso 1 1 calc R U . . .
C71 C 0.3104(3) 0.0120(3) 0.3207(2) 0.0323(9) Uani 1 1 d . . . . .
H71 H 0.261242 0.050466 0.343796 0.039 Uiso 1 1 calc R U . . .
C39 C 0.9664(3) -0.0746(3) 0.1206(2) 0.0259(8) Uani 1 1 d . . . . .
H39 H 0.917677 -0.030888 0.135976 0.031 Uiso 1 1 calc R U . . .
C49 C 0.7752(3) -0.2091(3) -0.0329(2) 0.0282(9) Uani 1 1 d . . . . .
H49 H 0.811500 -0.261426 -0.030422 0.034 Uiso 1 1 calc R U . . .
C19 C 0.9778(3) 0.1745(3) 0.3257(2) 0.0260(8) Uani 1 1 d . . . . .
C73 C 0.4841(3) -0.0465(2) 0.3140(2) 0.0248(8) Uani 1 1 d . . . . .
H73 H 0.554423 -0.047052 0.332335 0.030 Uiso 1 1 calc R U . . .
C72 C 0.4131(3) 0.0105(3) 0.3483(2) 0.0279(8) Uani 1 1 d . . . . .
H72 H 0.434467 0.047853 0.389960 0.034 Uiso 1 1 calc R U . . .
C55 C 0.6870(3) -0.3453(3) 0.0630(2) 0.0266(8) Uani 1 1 d . . . . .
H55 H 0.642817 -0.312669 0.036672 0.032 Uiso 1 1 calc R U . . .
C6 C 0.8071(3) 0.2344(2) 0.2061(2) 0.0250(8) Uani 1 1 d . . . . .
C37 C 0.6906(3) -0.1599(3) 0.3981(2) 0.0279(9) Uani 1 1 d . . . . .
H37 H 0.641678 -0.172258 0.359610 0.033 Uiso 1 1 calc R U . . .
C43 C 1.0045(3) -0.2255(3) 0.0836(2) 0.0284(9) Uani 1 1 d . . . . .
H43 H 0.982260 -0.284973 0.072360 0.034 Uiso 1 1 calc R U . . .
C57 C 0.4800(3) -0.1647(3) 0.0787(2) 0.0282(9) Uani 1 1 d . . . . .
H57 H 0.508859 -0.107080 0.089718 0.034 Uiso 1 1 calc R U . . .
C70 C 0.2794(3) -0.0417(3) 0.2602(2) 0.0342(10) Uani 1 1 d . . . . .
H70 H 0.209679 -0.039125 0.241285 0.041 Uiso 1 1 calc R U . . .
C69 C 0.3501(3) -0.1002(3) 0.2265(2) 0.0272(8) Uani 1 1 d . . . . .
H69 H 0.327743 -0.138126 0.185438 0.033 Uiso 1 1 calc R U . . .
C47 C 0.6983(3) -0.1084(3) -0.1013(2) 0.0338(10) Uani 1 1 d . . . . .
H47 H 0.681575 -0.091636 -0.145317 0.041 Uiso 1 1 calc R U . . .
C42 C 1.1100(3) -0.2012(3) 0.0768(2) 0.0356(10) Uani 1 1 d . . . . .
H42 H 1.159549 -0.244687 0.062599 0.043 Uiso 1 1 calc R U . . .
C52 C 0.8162(3) -0.4422(3) 0.1385(2) 0.0321(9) Uani 1 1 d . . . . .
H52 H 0.860590 -0.475351 0.164203 0.039 Uiso 1 1 calc R U . . .
C61 C 0.4372(3) -0.3037(3) 0.1122(2) 0.0334(9) Uani 1 1 d . . . . .
H61 H 0.437200 -0.341853 0.146037 0.040 Uiso 1 1 calc R U . . .
C7 C 0.5984(3) 0.2270(3) 0.3475(2) 0.0327(10) Uani 1 1 d . . . . .
H7 H 0.609431 0.163696 0.348596 0.039 Uiso 1 1 calc R U . . .
C27 C 1.0305(3) -0.1933(3) 0.2655(2) 0.0295(9) Uani 1 1 d . . . . .
H27 H 1.048604 -0.140277 0.249456 0.035 Uiso 1 1 calc R U . . .
C26 C 0.9311(3) -0.2032(2) 0.29408(19) 0.0230(8) Uani 1 1 d . . . . .
C28 C 1.1028(4) -0.2604(3) 0.2603(2) 0.0398(11) Uani 1 1 d . . . . .
H28 H 1.169032 -0.253218 0.240185 0.048 Uiso 1 1 calc R U . . .
C41 C 1.1433(3) -0.1151(3) 0.0905(2) 0.0366(11) Uani 1 1 d . . . . .
H41 H 1.215068 -0.099238 0.085354 0.044 Uiso 1 1 calc R U . . .
C36 C 0.6613(4) -0.1761(3) 0.4638(2) 0.0349(10) Uani 1 1 d . . . . .
H36 H 0.592552 -0.198802 0.469774 0.042 Uiso 1 1 calc R U . . .
C31 C 0.9075(4) -0.2827(3) 0.3179(2) 0.0339(10) Uani 1 1 d . . . . .
H31 H 0.841049 -0.291575 0.337189 0.041 Uiso 1 1 calc R U . . .
C34 C 0.8308(4) -0.1233(3) 0.5116(2) 0.0361(10) Uani 1 1 d . . . . .
H34 H 0.878408 -0.109391 0.550696 0.043 Uiso 1 1 calc R U . . .
C48 C 0.7503(3) -0.1846(3) -0.0975(2) 0.0325(9) Uani 1 1 d . . . . .
H48 H 0.769227 -0.220520 -0.138883 0.039 Uiso 1 1 calc R U . . .
C46 C 0.6705(3) -0.0564(3) -0.0412(2) 0.0321(9) Uani 1 1 d . . . . .
H46 H 0.634809 -0.003851 -0.043968 0.038 Uiso 1 1 calc R U . . .
C11 C 0.8226(4) 0.1368(3) 0.0917(2) 0.0357(10) Uani 1 1 d . . . . .
H11A H 0.759366 0.104067 0.101690 0.054 Uiso 1 1 calc R U . . .
H11B H 0.869800 0.097472 0.064151 0.054 Uiso 1 1 calc R U . . .
H11C H 0.802038 0.183359 0.065511 0.054 Uiso 1 1 calc R U . . .
C18 C 0.8795(3) 0.1629(3) 0.4777(2) 0.0336(9) Uani 1 1 d . . . . .
H18 H 0.945132 0.188175 0.467916 0.040 Uiso 1 1 calc R U . . .
C15 C 0.6877(4) 0.0889(3) 0.5084(2) 0.0371(10) Uani 1 1 d . . . . .
H15 H 0.622287 0.063648 0.518592 0.045 Uiso 1 1 calc R U . . .
C9 C 0.6218(4) 0.2765(3) 0.4214(2) 0.0440(12) Uani 1 1 d . . . . .
H9A H 0.695542 0.268724 0.435299 0.066 Uiso 1 1 calc R U . . .
H9B H 0.575256 0.253652 0.453963 0.066 Uiso 1 1 calc R U . . .
H9C H 0.609375 0.338663 0.421846 0.066 Uiso 1 1 calc R U . . .
C63 C 0.6121(4) -0.3333(3) 0.2592(2) 0.0344(10) Uani 1 1 d . . . . .
H63 H 0.670910 -0.328737 0.230893 0.041 Uiso 1 1 calc R U . . .
C2 C 0.6720(3) 0.2568(3) 0.2950(2) 0.0281(9) Uani 1 1 d . . . . .
C8 C 0.4815(4) 0.2382(3) 0.3255(3) 0.0462(12) Uani 1 1 d . . . . .
H8A H 0.468718 0.300059 0.324667 0.069 Uiso 1 1 calc R U . . .
H8B H 0.435444 0.216446 0.358872 0.069 Uiso 1 1 calc R U . . .
H8C H 0.466447 0.205249 0.279117 0.069 Uiso 1 1 calc R U . . .
C58 C 0.4342(3) -0.1927(3) 0.0122(2) 0.0347(10) Uani 1 1 d . . . . .
H58 H 0.433293 -0.154445 -0.021560 0.042 Uiso 1 1 calc R U . . .
C5 C 0.7953(4) 0.3203(3) 0.1957(2) 0.0393(11) Uani 1 1 d . . . . .
H5 H 0.835368 0.341899 0.161266 0.047 Uiso 1 1 calc R U . . .
C35 C 0.7318(4) -0.1593(3) 0.5197(2) 0.0371(10) Uani 1 1 d . . . . .
H35 H 0.712646 -0.172316 0.563826 0.045 Uiso 1 1 calc R U . . .
C40 C 1.0702(3) -0.0507(3) 0.1120(2) 0.0340(10) Uani 1 1 d . . . . .
H40 H 1.092116 0.008952 0.120695 0.041 Uiso 1 1 calc R U . . .
C60 C 0.3910(4) -0.3307(3) 0.0461(3) 0.0430(11) Uani 1 1 d . . . . .
H60 H 0.359358 -0.387385 0.035249 0.052 Uiso 1 1 calc R U . . .
C53 C 0.7309(4) -0.4830(3) 0.0982(2) 0.0385(11) Uani 1 1 d . . . . .
H53 H 0.717630 -0.543787 0.095982 0.046 Uiso 1 1 calc R U . . .
C54 C 0.6655(3) -0.4341(3) 0.0613(2) 0.0336(9) Uani 1 1 d . . . . .
H54 H 0.606050 -0.461176 0.034903 0.040 Uiso 1 1 calc R U . . .
C17 C 0.8458(4) 0.1734(3) 0.5462(2) 0.0443(12) Uani 1 1 d . . . . .
H17 H 0.888547 0.206016 0.582543 0.053 Uiso 1 1 calc R U . . .
C23 C 1.1607(3) 0.2043(3) 0.2979(2) 0.0409(11) Uani 1 1 d . . . . .
H23 H 1.225760 0.183531 0.280140 0.049 Uiso 1 1 calc R U . . .
C16 C 0.7508(4) 0.1366(3) 0.5611(2) 0.0451(12) Uani 1 1 d . . . . .
H16 H 0.728367 0.143881 0.607562 0.054 Uiso 1 1 calc R U . . .
C20 C 0.9679(4) 0.2647(3) 0.3472(2) 0.0394(11) Uani 1 1 d . . . . .
H20 H 0.902341 0.286786 0.362990 0.047 Uiso 1 1 calc R U . . .
C29 C 1.0777(4) -0.3370(3) 0.2845(3) 0.0453(12) Uani 1 1 d . . . . .
H29 H 1.127079 -0.382377 0.281434 0.054 Uiso 1 1 calc R U . . .
C12 C 0.9825(4) 0.2234(3) 0.1449(3) 0.0431(11) Uani 1 1 d . . . . .
H12A H 0.966038 0.268077 0.115864 0.065 Uiso 1 1 calc R U . . .
H12B H 1.029361 0.180987 0.120325 0.065 Uiso 1 1 calc R U . . .
H12C H 1.017435 0.250896 0.188656 0.065 Uiso 1 1 calc R U . . .
C30 C 0.9812(4) -0.3482(3) 0.3133(3) 0.0440(12) Uani 1 1 d . . . . .
H30 H 0.964922 -0.401136 0.330018 0.053 Uiso 1 1 calc R U . . .
C59 C 0.3907(4) -0.2753(3) -0.0042(2) 0.0425(11) Uani 1 1 d . . . . .
H59 H 0.360592 -0.294670 -0.049390 0.051 Uiso 1 1 calc R U . . .
C3 C 0.6661(4) 0.3437(3) 0.2832(3) 0.0418(12) Uani 1 1 d . . . . .
H3 H 0.619492 0.381704 0.309281 0.050 Uiso 1 1 calc R U . . .
C67 C 0.4485(4) -0.2794(3) 0.3036(3) 0.0408(11) Uani 1 1 d . . . . .
H67 H 0.393588 -0.238614 0.305212 0.049 Uiso 1 1 calc R U . . .
C64 C 0.6053(5) -0.4012(3) 0.2981(3) 0.0499(13) Uani 1 1 d . . . . .
H64 H 0.658289 -0.443747 0.295425 0.060 Uiso 1 1 calc R U . . .
C22 C 1.1500(4) 0.2923(4) 0.3207(3) 0.0524(14) Uani 1 1 d . . . . .
H22 H 1.207921 0.331902 0.319379 0.063 Uiso 1 1 calc R U . . .
C4 C 0.7277(4) 0.3752(3) 0.2335(3) 0.0482(13) Uani 1 1 d . . . . .
H4 H 0.722924 0.434093 0.225947 0.058 Uiso 1 1 calc R U . . .
C21 C 1.0551(4) 0.3222(3) 0.3455(3) 0.0551(14) Uani 1 1 d . . . . .
H21 H 1.048210 0.382589 0.361662 0.066 Uiso 1 1 calc R U . . .
C65 C 0.5201(5) -0.4067(4) 0.3412(3) 0.0608(16) Uani 1 1 d . . . . .
H65 H 0.515853 -0.452195 0.368696 0.073 Uiso 1 1 calc R U . . .
C66 C 0.4436(5) -0.3467(4) 0.3435(3) 0.0606(16) Uani 1 1 d . . . . .
H66 H 0.385832 -0.350635 0.372744 0.073 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N1 1.876(3) . ?
Ge1 Ni1 2.1994(7) . ?
Ge1 Br1 2.3802(9) . ?
Ni1 P2 2.2028(12) . ?
Ni1 P1 2.2079(12) . ?
Ni1 P3 2.2152(11) . ?
P1 C25 1.857(4) . ?
P1 C26 1.858(4) . ?
P1 C32 1.859(4) . ?
Si1 N1 1.762(3) . ?
Si1 C13 1.889(4) . ?
Si1 C25 1.891(4) . ?
Si1 C19 1.892(4) . ?
P3 C56 1.849(4) . ?
P3 C68 1.854(4) . ?
P3 C62 1.855(4) . ?
P2 C50 1.848(4) . ?
P2 C38 1.854(4) . ?
P2 C44 1.857(4) . ?
N1 C1 1.455(5) . ?
C10 C6 1.516(5) . ?
C10 C12 1.535(6) . ?
C10 C11 1.539(6) . ?
C1 C2 1.410(5) . ?
C1 C6 1.434(5) . ?
C68 C73 1.399(5) . ?
C68 C69 1.404(5) . ?
C38 C43 1.402(5) . ?
C38 C39 1.407(5) . ?
C44 C45 1.384(5) . ?
C44 C49 1.406(5) . ?
C50 C55 1.389(5) . ?
C50 C51 1.414(5) . ?
C32 C37 1.384(5) . ?
C32 C33 1.399(5) . ?
C51 C52 1.391(5) . ?
C14 C15 1.391(6) . ?
C14 C13 1.401(6) . ?
C56 C57 1.386(5) . ?
C56 C61 1.404(5) . ?
C13 C18 1.407(6) . ?
C62 C67 1.389(6) . ?
C62 C63 1.396(6) . ?
C33 C34 1.397(6) . ?
C24 C23 1.398(6) . ?
C24 C19 1.411(6) . ?
C45 C46 1.393(5) . ?
C71 C70 1.377(6) . ?
C71 C72 1.395(6) . ?
C39 C40 1.382(6) . ?
C49 C48 1.396(5) . ?
C19 C20 1.411(6) . ?
C73 C72 1.393(5) . ?
C55 C54 1.395(6) . ?
C6 C5 1.390(6) . ?
C37 C36 1.402(6) . ?
C43 C42 1.399(6) . ?
C57 C58 1.403(6) . ?
C70 C69 1.400(6) . ?
C47 C48 1.379(6) . ?
C47 C46 1.380(6) . ?
C42 C41 1.378(7) . ?
C52 C53 1.396(6) . ?
C61 C60 1.397(6) . ?
C7 C2 1.524(5) . ?
C7 C9 1.541(6) . ?
C7 C8 1.549(6) . ?
C27 C28 1.398(6) . ?
C27 C26 1.409(6) . ?
C26 C31 1.412(5) . ?
C28 C29 1.378(7) . ?
C41 C40 1.406(7) . ?
C36 C35 1.373(6) . ?
C31 C30 1.391(6) . ?
C34 C35 1.386(6) . ?
C18 C17 1.403(6) . ?
C15 C16 1.389(7) . ?
C63 C64 1.390(6) . ?
C2 C3 1.406(6) . ?
C58 C59 1.373(7) . ?
C5 C4 1.376(6) . ?
C60 C59 1.396(7) . ?
C53 C54 1.389(7) . ?
C17 C16 1.380(7) . ?
C23 C22 1.385(8) . ?
C20 C21 1.410(6) . ?
C29 C30 1.382(7) . ?
C3 C4 1.401(6) . ?
C67 C66 1.394(6) . ?
C64 C65 1.399(8) . ?
C22 C21 1.377(8) . ?
C65 C66 1.358(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ge1 Ni1 132.40(9) . . ?
N1 Ge1 Br1 98.84(9) . . ?
Ni1 Ge1 Br1 128.46(3) . . ?
Ge1 Ni1 P2 114.52(4) . . ?
Ge1 Ni1 P1 97.33(4) . . ?
P2 Ni1 P1 109.01(4) . . ?
Ge1 Ni1 P3 103.83(4) . . ?
P2 Ni1 P3 108.94(5) . . ?
P1 Ni1 P3 122.87(4) . . ?
C25 P1 C26 101.55(17) . . ?
C25 P1 C32 104.09(17) . . ?
C26 P1 C32 96.51(17) . . ?
C25 P1 Ni1 111.75(12) . . ?
C26 P1 Ni1 117.59(13) . . ?
C32 P1 Ni1 122.36(13) . . ?
N1 Si1 C13 111.85(16) . . ?
N1 Si1 C25 110.58(16) . . ?
C13 Si1 C25 110.15(17) . . ?
N1 Si1 C19 109.99(16) . . ?
C13 Si1 C19 107.71(18) . . ?
C25 Si1 C19 106.37(17) . . ?
C56 P3 C68 100.63(17) . . ?
C56 P3 C62 101.96(17) . . ?
C68 P3 C62 100.66(17) . . ?
C56 P3 Ni1 117.71(12) . . ?
C68 P3 Ni1 115.47(12) . . ?
C62 P3 Ni1 117.58(13) . . ?
C50 P2 C38 105.28(17) . . ?
C50 P2 C44 102.72(17) . . ?
C38 P2 C44 96.00(16) . . ?
C50 P2 Ni1 111.28(12) . . ?
C38 P2 Ni1 117.75(13) . . ?
C44 P2 Ni1 121.42(12) . . ?
C1 N1 Si1 117.6(2) . . ?
C1 N1 Ge1 122.9(2) . . ?
Si1 N1 Ge1 118.78(16) . . ?
P1 C25 Si1 123.98(19) . . ?
C6 C10 C12 113.8(4) . . ?
C6 C10 C11 110.9(3) . . ?
C12 C10 C11 109.5(3) . . ?
C2 C1 C6 120.6(3) . . ?
C2 C1 N1 121.3(3) . . ?
C6 C1 N1 118.0(3) . . ?
C73 C68 C69 118.4(3) . . ?
C73 C68 P3 118.5(3) . . ?
C69 C68 P3 123.1(3) . . ?
C43 C38 C39 118.3(3) . . ?
C43 C38 P2 125.0(3) . . ?
C39 C38 P2 116.5(3) . . ?
C45 C44 C49 118.6(3) . . ?
C45 C44 P2 120.4(3) . . ?
C49 C44 P2 120.9(3) . . ?
C55 C50 C51 118.7(3) . . ?
C55 C50 P2 120.7(3) . . ?
C51 C50 P2 119.9(3) . . ?
C37 C32 C33 118.7(3) . . ?
C37 C32 P1 118.9(3) . . ?
C33 C32 P1 122.1(3) . . ?
C52 C51 C50 120.1(4) . . ?
C15 C14 C13 122.0(4) . . ?
C57 C56 C61 118.9(4) . . ?
C57 C56 P3 117.7(3) . . ?
C61 C56 P3 123.4(3) . . ?
C14 C13 C18 117.4(4) . . ?
C14 C13 Si1 120.9(3) . . ?
C18 C13 Si1 121.6(3) . . ?
C67 C62 C63 118.8(4) . . ?
C67 C62 P3 123.2(3) . . ?
C63 C62 P3 117.9(3) . . ?
C34 C33 C32 120.3(4) . . ?
C23 C24 C19 121.4(4) . . ?
C44 C45 C46 120.6(4) . . ?
C70 C71 C72 120.6(4) . . ?
C40 C39 C38 121.3(4) . . ?
C48 C49 C44 120.4(4) . . ?
C24 C19 C20 117.4(4) . . ?
C24 C19 Si1 122.3(3) . . ?
C20 C19 Si1 120.3(3) . . ?
C72 C73 C68 121.5(4) . . ?
C73 C72 C71 119.0(4) . . ?
C50 C55 C54 121.0(4) . . ?
C5 C6 C1 118.0(4) . . ?
C5 C6 C10 119.3(3) . . ?
C1 C6 C10 122.7(3) . . ?
C32 C37 C36 120.7(4) . . ?
C42 C43 C38 120.1(4) . . ?
C56 C57 C58 120.9(4) . . ?
C71 C70 C69 120.4(4) . . ?
C70 C69 C68 120.1(4) . . ?
C48 C47 C46 119.9(4) . . ?
C41 C42 C43 121.0(4) . . ?
C51 C52 C53 120.4(4) . . ?
C60 C61 C56 119.7(4) . . ?
C2 C7 C9 111.9(4) . . ?
C2 C7 C8 110.8(4) . . ?
C9 C7 C8 109.7(4) . . ?
C28 C27 C26 121.0(4) . . ?
C27 C26 C31 117.8(4) . . ?
C27 C26 P1 122.7(3) . . ?
C31 C26 P1 119.5(3) . . ?
C29 C28 C27 119.7(4) . . ?
C42 C41 C40 119.5(4) . . ?
C35 C36 C37 120.1(4) . . ?
C30 C31 C26 120.3(4) . . ?
C35 C34 C33 120.1(4) . . ?
C47 C48 C49 120.0(4) . . ?
C47 C46 C45 120.4(4) . . ?
C17 C18 C13 120.7(4) . . ?
C16 C15 C14 119.4(4) . . ?
C64 C63 C62 120.5(4) . . ?
C3 C2 C1 118.4(4) . . ?
C3 C2 C7 117.5(4) . . ?
C1 C2 C7 124.2(3) . . ?
C59 C58 C57 120.2(4) . . ?
C4 C5 C6 122.4(4) . . ?
C36 C35 C34 120.0(4) . . ?
C39 C40 C41 119.8(4) . . ?
C59 C60 C61 120.7(4) . . ?
C54 C53 C52 119.6(4) . . ?
C53 C54 C55 120.1(4) . . ?
C16 C17 C18 120.1(4) . . ?
C22 C23 C24 120.3(4) . . ?
C17 C16 C15 120.4(4) . . ?
C21 C20 C19 120.2(4) . . ?
C30 C29 C28 120.4(4) . . ?
C29 C30 C31 120.7(4) . . ?
C58 C59 C60 119.5(4) . . ?
C4 C3 C2 121.1(4) . . ?
C62 C67 C66 120.2(5) . . ?
C63 C64 C65 119.8(5) . . ?
C21 C22 C23 119.6(4) . . ?
C5 C4 C3 119.5(4) . . ?
C22 C21 C20 121.1(5) . . ?
C66 C65 C64 119.7(4) . . ?
C65 C66 C67 121.0(5) . . ?

_refine_diff_density_max         0.882
_refine_diff_density_min         -1.882
_refine_diff_density_rms         0.107


