################################################################################

data_paper

_publ_contact_author
;
Alejandro Pérez Luna
;
_publ_contact_author_phone      '+33 1 44 27 55 71'
_publ_contact_author_email      'alejandro.perez_luna@sorbonne-universite.fr'
_publ_section_title
; 
Radical Germylzincation of α-Heteroatom-substituted Alkynes
;

loop_
_publ_author_name
_publ_author_address
'Karen de la Vega-Hernández'
;
Institut Parisien de Chimie Moléculaire, CNRS UMR 8232, Sorbonne Université
4 place Jussieu, 75252 Paris Cedex 05, France
;
'Elise Romain'
;
Institut Parisien de Chimie Moléculaire, CNRS UMR 8232, Sorbonne Université
4 place Jussieu, 75252 Paris Cedex 05, France
;
'Anais Coffinet'
;
Institut Parisien de Chimie Moléculaire, CNRS UMR 8232, Sorbonne Université
4 place Jussieu, 75252 Paris Cedex 05, France
;
'Kajetan Bijouard'
;
Institut Parisien de Chimie Moléculaire, CNRS UMR 8232, Sorbonne Université
4 place Jussieu, 75252 Paris Cedex 05, France
;
'Geoffrey Gontard'
;
Institut Parisien de Chimie Moléculaire, CNRS UMR 8232, Sorbonne Université
4 place Jussieu, 75252 Paris Cedex 05, France
;
'Fabrice Chemla'
;
Institut Parisien de Chimie Moléculaire, CNRS UMR 8232, Sorbonne Université
4 place Jussieu, 75252 Paris Cedex 05, France
;
'Franck Ferreira'
;
Institut Parisien de Chimie Moléculaire, CNRS UMR 8232, Sorbonne Université
4 place Jussieu, 75252 Paris Cedex 05, France
;
'Olivier Jackowski'
;
Institut Parisien de Chimie Moléculaire, CNRS UMR 8232, Sorbonne Université
4 place Jussieu, 75252 Paris Cedex 05, France
;
'Alejandro Pérez Luna'
;
Institut Parisien de Chimie Moléculaire, CNRS UMR 8232, Sorbonne Université
4 place Jussieu, 75252 Paris Cedex 05, France
;

################################################################################

data_Compound_12
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_formula_moiety          'C36 H31 Ge N O2'
_chemical_formula_sum             'C36 H31 Ge N O2'
_chemical_formula_weight          582.21

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0181   0.0091
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0311   0.0180
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0492   0.0322
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ge'  'Ge'  -1.0885   0.8855
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       tetragonal
_space_group_IT_number            92
_space_group_name_H-M_alt         'P 41 21 2'
_space_group_name_Hall            'P 4abw 2nw'
 
_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'
 '-y+1/2, x+1/2, z+1/4'
 'y+1/2, -x+1/2, z+3/4'
 '-x+1/2, y+1/2, -z+1/4'
 'x+1/2, -y+1/2, -z+3/4'
 'y, x, -z'
 '-y, -x, -z+1/2'
 
_cell_length_a                    9.5716(4)
_cell_length_b                    9.5716(4)
_cell_length_c                    64.226(3)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      5884.1(6)
_cell_formula_units_Z             8
_cell_measurement_temperature     200(1)
_cell_measurement_reflns_used     9942
_cell_measurement_theta_min       5.07
_cell_measurement_theta_max       66.64
 
_exptl_crystal_description        'fragment'
_exptl_crystal_colour             'colourless'
_exptl_crystal_density_method     'not measured'
_exptl_crystal_size_max           0.15
_exptl_crystal_size_mid           0.15
_exptl_crystal_size_min           0.05
_exptl_crystal_density_diffrn     1.314          
_exptl_crystal_F_000              2416
_exptl_absorpt_coefficient_mu     1.662
_exptl_absorpt_correction_type    numerical 
_exptl_absorpt_correction_T_min   0.738
_exptl_absorpt_correction_T_max   0.867
_exptl_absorpt_process_details     
; 
 SADABS : Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
; 
 
_diffrn_ambient_temperature       200(1)
_diffrn_radiation_wavelength      1.54178
_diffrn_radiation_type            CuK\a
_diffrn_radiation_source          'micro-source'
_diffrn_measurement_device_type   'Bruker APEX-II CCD'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_reflns_number             41850
_diffrn_reflns_av_unetI/netI      0.0437
_diffrn_reflns_av_R_equivalents   0.0744
_diffrn_reflns_limit_h_min        -8
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -11
_diffrn_reflns_limit_k_max        11
_diffrn_reflns_limit_l_min        -76
_diffrn_reflns_limit_l_max        76
_diffrn_reflns_theta_min          4.671
_diffrn_reflns_theta_max          66.656
_diffrn_reflns_theta_full         66.500
_diffrn_measured_fraction_theta_max   0.998
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    0.998
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   0.996
_diffrn_reflns_point_group_measured_fraction_full  0.998
_reflns_number_total              5180
_reflns_number_gt                 5003
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.632
_reflns_Friedel_fraction_max      0.993
_reflns_Friedel_fraction_full     0.995
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'Bruker APEX2'
_computing_cell_refinement        'Bruker SAINT'
_computing_data_reduction         'Bruker SAINT'
_computing_structure_solution     'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement   'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics     'SXGRAPH (Farrugia, 2012)'
_computing_publication_material   'WinGX (Farrugia, 2012)'

_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0394P)²+1.4078P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      dual
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_abs_structure_details
;
 Flack x determined using 1901 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack    -0.005(12)
_chemical_absolute_configuration  ad
_refine_ls_number_reflns          5180
_refine_ls_number_parameters      361
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0318
_refine_ls_R_factor_gt            0.0307
_refine_ls_wR_factor_ref          0.0780
_refine_ls_wR_factor_gt           0.0773
_refine_ls_goodness_of_fit_ref    1.065
_refine_ls_restrained_S_all       1.065
_refine_ls_shift/su_max           0.002
_refine_ls_shift/su_mean          0.000
_refine_diff_density_max          0.349
_refine_diff_density_min         -0.347
_refine_diff_density_rms          0.053
 
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 0.45420(3) 0.24666(3) 0.58221(2) 0.02141(11) Uani 1 1 d . . . . .
O1 O -0.0696(3) 0.0318(3) 0.53166(4) 0.0447(6) Uani 1 1 d . . . . .
O2 O 0.0957(3) -0.0977(3) 0.54724(5) 0.0574(8) Uani 1 1 d . . . . .
N1 N 0.0780(3) 0.1404(3) 0.55314(4) 0.0263(5) Uani 1 1 d . . . . .
C1 C 0.0412(4) 0.0144(3) 0.54451(5) 0.0370(8) Uani 1 1 d . . . . .
C2 C -0.1154(3) 0.1752(4) 0.53312(5) 0.0339(7) Uani 1 1 d . . . . .
H2A H -0.1953 0.1839 0.5428 0.041 Uiso 1 1 calc R U . . .
H2B H -0.1439 0.2111 0.5193 0.041 Uiso 1 1 calc R U . . .
C3 C 0.0108(3) 0.2543(3) 0.54128(4) 0.0242(6) Uani 1 1 d . . . . .
H3 H -0.0187 0.3317 0.5508 0.029 Uiso 1 1 calc R U . . .
C4 C 0.1098(3) 0.3091(4) 0.52431(4) 0.0330(7) Uani 1 1 d . . . . .
H4A H 0.1943 0.3484 0.5310 0.040 Uiso 1 1 calc R U . . .
H4B H 0.1395 0.2300 0.5154 0.040 Uiso 1 1 calc R U . . .
C5 C 0.0435(3) 0.4197(4) 0.51078(4) 0.0327(7) Uani 1 1 d . . . . .
C6 C 0.0465(4) 0.5593(4) 0.51673(5) 0.0385(7) Uani 1 1 d . . . . .
H6 H 0.0927 0.5855 0.5292 0.046 Uiso 1 1 calc R U . . .
C7 C -0.0178(4) 0.6616(4) 0.50449(6) 0.0461(9) Uani 1 1 d . . . . .
H7 H -0.0160 0.7566 0.5088 0.055 Uiso 1 1 calc R U . . .
C8 C -0.0838(4) 0.6248(4) 0.48625(5) 0.0473(9) Uani 1 1 d . . . . .
H8 H -0.1270 0.6943 0.4779 0.057 Uiso 1 1 calc R U . . .
C9 C -0.0869(4) 0.4861(5) 0.48015(5) 0.0461(9) Uani 1 1 d . . . . .
H9 H -0.1328 0.4603 0.4676 0.055 Uiso 1 1 calc R U . . .
C10 C -0.0232(4) 0.3851(4) 0.49225(4) 0.0386(8) Uani 1 1 d . . . . .
H10 H -0.0251 0.2904 0.4878 0.046 Uiso 1 1 calc R U . . .
C11 C 0.2049(3) 0.1493(3) 0.56407(4) 0.0237(6) Uani 1 1 d . . . . .
H11 H 0.2606 0.0671 0.5643 0.028 Uiso 1 1 calc R U . . .
C12 C 0.2561(3) 0.2597(3) 0.57411(4) 0.0228(5) Uani 1 1 d . . . . .
C13 C 0.1813(3) 0.3934(3) 0.57755(4) 0.0241(6) Uani 1 1 d . . . . .
C14 C 0.0559(3) 0.3964(3) 0.58822(4) 0.0315(7) Uani 1 1 d . . . . .
H14 H 0.0146 0.3110 0.5926 0.038 Uiso 1 1 calc R U . . .
C15 C -0.0107(4) 0.5210(4) 0.59266(5) 0.0434(9) Uani 1 1 d . . . . .
H15 H -0.0966 0.5207 0.6001 0.052 Uiso 1 1 calc R U . . .
C16 C 0.0474(4) 0.6453(4) 0.58634(6) 0.0484(9) Uani 1 1 d . . . . .
H16 H 0.0014 0.7309 0.5894 0.058 Uiso 1 1 calc R U . . .
C17 C 0.1722(4) 0.6463(4) 0.57560(6) 0.0454(9) Uani 1 1 d . . . . .
H17 H 0.2118 0.7323 0.5712 0.054 Uiso 1 1 calc R U . . .
C18 C 0.2402(4) 0.5204(3) 0.57126(5) 0.0332(7) Uani 1 1 d . . . . .
H18 H 0.3267 0.5210 0.5640 0.040 Uiso 1 1 calc R U . . .
C19 C 0.5563(3) 0.3318(3) 0.55896(4) 0.0251(6) Uani 1 1 d . . . . .
C20 C 0.6581(4) 0.4331(3) 0.56184(5) 0.0334(7) Uani 1 1 d . . . . .
H20 H 0.6875 0.4563 0.5755 0.040 Uiso 1 1 calc R U . . .
C21 C 0.7175(4) 0.5011(4) 0.54489(6) 0.0431(8) Uani 1 1 d . . . . .
H21 H 0.7884 0.5690 0.5470 0.052 Uiso 1 1 calc R U . . .
C22 C 0.6732(4) 0.4697(4) 0.52492(5) 0.0468(9) Uani 1 1 d . . . . .
H22 H 0.7116 0.5184 0.5134 0.056 Uiso 1 1 calc R U . . .
C23 C 0.5736(4) 0.3683(4) 0.52176(5) 0.0418(8) Uani 1 1 d . . . . .
H23 H 0.5450 0.3455 0.5080 0.050 Uiso 1 1 calc R U . . .
C24 C 0.5148(4) 0.2992(4) 0.53863(4) 0.0327(7) Uani 1 1 d . . . . .
H24 H 0.4460 0.2293 0.5364 0.039 Uiso 1 1 calc R U . . .
C25 C 0.4992(3) 0.3476(3) 0.60783(4) 0.0236(6) Uani 1 1 d . . . . .
C26 C 0.4028(3) 0.4269(3) 0.61882(4) 0.0294(7) Uani 1 1 d . . . . .
H26 H 0.3085 0.4308 0.6143 0.035 Uiso 1 1 calc R U . . .
C27 C 0.4434(4) 0.5008(4) 0.63645(5) 0.0353(7) Uani 1 1 d . . . . .
H27 H 0.3760 0.5531 0.6440 0.042 Uiso 1 1 calc R U . . .
C28 C 0.5803(4) 0.4989(4) 0.64305(5) 0.0361(8) Uani 1 1 d . . . . .
H28 H 0.6077 0.5513 0.6549 0.043 Uiso 1 1 calc R U . . .
C29 C 0.6771(4) 0.4208(4) 0.63236(5) 0.0405(8) Uani 1 1 d . . . . .
H29 H 0.7717 0.4193 0.6368 0.049 Uiso 1 1 calc R U . . .
C30 C 0.6365(4) 0.3439(4) 0.61498(5) 0.0378(7) Uani 1 1 d . . . . .
H30 H 0.7034 0.2882 0.6079 0.045 Uiso 1 1 calc R U . . .
C31 C 0.4988(3) 0.0487(3) 0.58540(4) 0.0244(6) Uani 1 1 d . . . . .
C32 C 0.4369(3) -0.0252(4) 0.60169(5) 0.0342(7) Uani 1 1 d . . . . .
H32 H 0.3818 0.0233 0.6116 0.041 Uiso 1 1 calc R U . . .
C33 C 0.4548(4) -0.1685(4) 0.60356(5) 0.0419(8) Uani 1 1 d . . . . .
H33 H 0.4102 -0.2180 0.6145 0.050 Uiso 1 1 calc R U . . .
C34 C 0.5371(4) -0.2384(4) 0.58950(6) 0.0466(9) Uani 1 1 d . . . . .
H34 H 0.5489 -0.3366 0.5907 0.056 Uiso 1 1 calc R U . . .
C35 C 0.6021(5) -0.1670(4) 0.57385(5) 0.0480(10) Uani 1 1 d . . . . .
H35 H 0.6609 -0.2155 0.5644 0.058 Uiso 1 1 calc R U . . .
C36 C 0.5827(4) -0.0234(4) 0.57167(4) 0.0350(7) Uani 1 1 d . . . . .
H36 H 0.6278 0.0251 0.5607 0.042 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 C31 1.953(3) . ?
Ge1 C25 1.956(3) . ?
Ge1 C19 1.962(3) . ?
Ge1 C12 1.970(3) . ?
O1 C1 1.354(4) . ?
O1 C2 1.445(4) . ?
O2 C1 1.206(4) . ?
N1 C1 1.373(4) . ?
N1 C11 1.406(4) . ?
N1 C3 1.478(4) . ?
C2 C3 1.519(4) . ?
C3 C4 1.536(4) . ?
C4 C5 1.510(4) . ?
C5 C6 1.390(5) . ?
C5 C10 1.391(5) . ?
C6 C7 1.399(5) . ?
C7 C8 1.376(6) . ?
C8 C9 1.385(6) . ?
C9 C10 1.382(5) . ?
C11 C12 1.332(4) . ?
C12 C13 1.483(4) . ?
C13 C14 1.383(5) . ?
C13 C18 1.399(4) . ?
C14 C15 1.382(5) . ?
C15 C16 1.375(6) . ?
C16 C17 1.379(6) . ?
C17 C18 1.398(5) . ?
C19 C20 1.387(5) . ?
C19 C24 1.399(4) . ?
C20 C21 1.390(5) . ?
C21 C22 1.384(5) . ?
C22 C23 1.376(6) . ?
C23 C24 1.389(5) . ?
C25 C26 1.387(4) . ?
C25 C30 1.393(4) . ?
C26 C27 1.390(4) . ?
C27 C28 1.378(5) . ?
C28 C29 1.374(5) . ?
C29 C30 1.392(5) . ?
C31 C36 1.378(4) . ?
C31 C32 1.395(4) . ?
C32 C33 1.387(5) . ?
C33 C34 1.373(5) . ?
C34 C35 1.365(6) . ?
C35 C36 1.394(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
C31 Ge1 C25 110.06(11) . . ?
C31 Ge1 C19 111.95(12) . . ?
C25 Ge1 C19 109.00(12) . . ?
C31 Ge1 C12 107.44(12) . . ?
C25 Ge1 C12 113.73(12) . . ?
C19 Ge1 C12 104.60(11) . . ?
C1 O1 C2 108.4(2) . . ?
C1 N1 C11 118.4(3) . . ?
C1 N1 C3 109.2(2) . . ?
C11 N1 C3 126.1(2) . . ?
O2 C1 O1 122.5(3) . . ?
O2 C1 N1 127.7(3) . . ?
O1 C1 N1 109.8(3) . . ?
O1 C2 C3 104.7(2) . . ?
N1 C3 C2 99.0(2) . . ?
N1 C3 C4 110.5(2) . . ?
C2 C3 C4 114.6(2) . . ?
C5 C4 C3 112.9(3) . . ?
C6 C5 C10 118.3(3) . . ?
C6 C5 C4 120.5(3) . . ?
C10 C5 C4 121.2(3) . . ?
C5 C6 C7 120.6(3) . . ?
C8 C7 C6 120.1(4) . . ?
C7 C8 C9 119.7(3) . . ?
C10 C9 C8 120.2(3) . . ?
C9 C10 C5 121.1(4) . . ?
C12 C11 N1 127.4(3) . . ?
C11 C12 C13 125.4(3) . . ?
C11 C12 Ge1 115.6(2) . . ?
C13 C12 Ge1 118.7(2) . . ?
C14 C13 C18 118.3(3) . . ?
C14 C13 C12 120.7(3) . . ?
C18 C13 C12 120.8(3) . . ?
C15 C14 C13 121.4(3) . . ?
C16 C15 C14 120.0(3) . . ?
C15 C16 C17 120.2(3) . . ?
C16 C17 C18 119.8(4) . . ?
C17 C18 C13 120.3(3) . . ?
C20 C19 C24 118.7(3) . . ?
C20 C19 Ge1 122.6(2) . . ?
C24 C19 Ge1 118.4(2) . . ?
C19 C20 C21 120.7(3) . . ?
C22 C21 C20 120.0(3) . . ?
C23 C22 C21 120.1(3) . . ?
C22 C23 C24 120.1(3) . . ?
C23 C24 C19 120.4(3) . . ?
C26 C25 C30 118.2(3) . . ?
C26 C25 Ge1 123.5(2) . . ?
C30 C25 Ge1 118.2(2) . . ?
C25 C26 C27 120.5(3) . . ?
C28 C27 C26 120.6(3) . . ?
C29 C28 C27 119.7(3) . . ?
C28 C29 C30 120.0(3) . . ?
C29 C30 C25 121.0(3) . . ?
C36 C31 C32 118.3(3) . . ?
C36 C31 Ge1 123.1(2) . . ?
C32 C31 Ge1 118.5(2) . . ?
C33 C32 C31 120.9(3) . . ?
C34 C33 C32 119.7(3) . . ?
C35 C34 C33 120.1(3) . . ?
C34 C35 C36 120.4(3) . . ?
C31 C36 C35 120.5(3) . . ?



################################################################################

data_Compound_14

_audit_creation_date              2017-07-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number      '2014/7'
_chemical_formula_moiety          'C34 H29 Ge N O2'
_chemical_formula_sum             'C34 H29 Ge N O2'
_chemical_formula_weight          556.17
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'
 'Ge' 'Ge' 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system       'monoclinic'
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 1 21/c 1'
_space_group_name_Hall            '-P 2ybc'
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                    10.4058(3)
_cell_length_b                    20.8929(7)
_cell_length_c                    13.6211(5)
_cell_angle_alpha                 90
_cell_angle_beta                  111.976(2)
_cell_angle_gamma                 90
_cell_volume                      2746.16(16)
_cell_formula_units_Z             4
_cell_measurement_reflns_used     9898
_cell_measurement_temperature     200
_cell_measurement_theta_max       30.06
_cell_measurement_theta_min       2.32
_exptl_absorpt_coefficient_mu     1.147
_exptl_absorpt_correction_T_max   0.7460
_exptl_absorpt_correction_T_min   0.6786
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_process_details    'SADABS-2014/5 - Bruker AXS'
_exptl_crystal_colour             colourless
_exptl_crystal_density_diffrn     1.345
_exptl_crystal_density_method     'not measured'
_exptl_crystal_description        block
_exptl_crystal_F_000              1152
_exptl_crystal_size_max           0.21
_exptl_crystal_size_mid           0.17
_exptl_crystal_size_min           0.17
_diffrn_reflns_av_R_equivalents   0.0182
_diffrn_reflns_av_unetI/netI      0.0152
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_k_max        29
_diffrn_reflns_limit_k_min        -23
_diffrn_reflns_limit_l_max        11
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_number             38870
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full         25.242
_diffrn_reflns_theta_max          30.164
_diffrn_reflns_theta_min          1.884
_diffrn_ambient_temperature       200
_diffrn_detector_area_resol_mean  8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type   'Bruker APEX-II CCD'
_diffrn_measurement_method        'ω and φ scans'
_diffrn_radiation_monochromator   graphite
_diffrn_radiation_type            MoK\a
_diffrn_radiation_wavelength      0.71073
_diffrn_source                    'sealed tube'
_reflns_number_gt                 6930
_reflns_number_total              8095
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;
_reflns_threshold_expression      'I > 2σ(I)'
_computing_data_collection        'Bruker APEX2'
_computing_cell_refinement        'Bruker SAINT'
_computing_data_reduction         'Bruker SAINT'
_computing_molecular_graphics     'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material   'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement   'ShelXL (Sheldrick, 2015)'
_computing_structure_solution     'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max          0.384
_refine_diff_density_min          -0.280
_refine_diff_density_rms          0.048
_refine_ls_extinction_method      none
_refine_ls_goodness_of_fit_ref    1.021
_refine_ls_hydrogen_treatment     constr
_refine_ls_matrix_type            full
_refine_ls_number_parameters      344
_refine_ls_number_reflns          8095
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0334
_refine_ls_R_factor_gt            0.0255
_refine_ls_restrained_S_all       1.021
_refine_ls_shift/su_max           0.003
_refine_ls_shift/su_mean          0.000
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0321P)²+1.0920P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme       calc
_refine_ls_wR_factor_gt           0.0635
_refine_ls_wR_factor_ref          0.0674
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22),
  C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31),
 C32(H32), C33(H33), C34(H34)
2.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens    geom
_atom_sites_solution_primary      dual
_atom_sites_solution_secondary    difmap
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 0.26233(2) 0.37583(2) 0.40837(2) 0.01962(4) Uani 1 1 d . . . . .
 O1 O 0.38565(10) 0.44003(5) 0.08681(7) 0.02917(19) Uani 1 1 d . . . . .
 O2 O 0.54400(10) 0.37137(5) 0.06974(7) 0.0294(2) Uani 1 1 d . . . . .
 N1 N 0.49154(10) 0.36558(5) 0.21472(8) 0.0222(2) Uani 1 1 d . . . . .
 C1 C 0.42372(12) 0.36847(5) 0.36931(9) 0.0201(2) Uani 1 1 d . . . . .
 C2 C 0.39947(12) 0.37853(6) 0.26662(9) 0.0215(2) Uani 1 1 d . . . . .
 H2 H 0.3118 0.3961 0.2247 0.026 Uiso 1 1 calc R . . . .
 C3 C 0.46624(12) 0.39616(6) 0.11984(9) 0.0229(2) Uani 1 1 d . . . . .
 C4 C 0.52481(17) 0.40088(8) -0.03047(11) 0.0373(3) Uani 1 1 d . . . . .
 H4A H 0.4262 0.4002 -0.0759 0.056 Uiso 1 1 calc GR . . . .
 H4B H 0.5777 0.3772 -0.0649 0.056 Uiso 1 1 calc GR . . . .
 H4C H 0.5574 0.4453 -0.0187 0.056 Uiso 1 1 calc GR . . . .
 C5 C 0.56094(11) 0.34942(6) 0.44930(9) 0.0199(2) Uani 1 1 d . . . . .
 C6 C 0.58570(13) 0.28807(6) 0.49285(9) 0.0242(2) Uani 1 1 d . . . . .
 H6 H 0.5127 0.2576 0.4733 0.029 Uiso 1 1 calc R . . . .
 C7 C 0.71589(14) 0.27129(7) 0.56432(10) 0.0306(3) Uani 1 1 d . . . . .
 H7 H 0.7322 0.2291 0.5922 0.037 Uiso 1 1 calc R . . . .
 C8 C 0.82243(14) 0.31571(8) 0.59531(10) 0.0330(3) Uani 1 1 d . . . . .
 H8 H 0.9117 0.3040 0.6441 0.040 Uiso 1 1 calc R . . . .
 C9 C 0.79849(14) 0.37704(7) 0.55515(11) 0.0315(3) Uani 1 1 d . . . . .
 H9 H 0.8710 0.4078 0.5773 0.038 Uiso 1 1 calc R . . . .
 C10 C 0.66859(13) 0.39409(6) 0.48239(10) 0.0262(2) Uani 1 1 d . . . . .
 H10 H 0.6529 0.4364 0.4550 0.031 Uiso 1 1 calc R . . . .
 C11 C 0.58262(12) 0.31077(6) 0.24733(9) 0.0206(2) Uani 1 1 d . . . . .
 C12 C 0.52557(13) 0.25017(6) 0.23381(10) 0.0263(2) Uani 1 1 d . . . . .
 H12 H 0.4284 0.2446 0.1987 0.032 Uiso 1 1 calc R . . . .
 C13 C 0.61116(16) 0.19744(7) 0.27184(11) 0.0330(3) Uani 1 1 d . . . . .
 H13 H 0.5725 0.1556 0.2628 0.040 Uiso 1 1 calc R . . . .
 C14 C 0.75224(16) 0.20574(7) 0.32279(11) 0.0346(3) Uani 1 1 d . . . . .
 H14 H 0.8104 0.1697 0.3501 0.041 Uiso 1 1 calc R . . . .
 C15 C 0.80892(14) 0.26632(7) 0.33411(11) 0.0315(3) Uani 1 1 d . . . . .
 H15 H 0.9063 0.2717 0.3681 0.038 Uiso 1 1 calc R . . . .
 C16 C 0.72468(12) 0.31933(6) 0.29620(9) 0.0244(2) Uani 1 1 d . . . . .
 H16 H 0.7638 0.3610 0.3036 0.029 Uiso 1 1 calc R . . . .
 C17 C 0.29046(12) 0.42509(6) 0.53605(9) 0.0223(2) Uani 1 1 d . . . . .
 C18 C 0.17387(14) 0.44646(7) 0.55414(11) 0.0311(3) Uani 1 1 d . . . . .
 H18 H 0.0843 0.4400 0.5014 0.037 Uiso 1 1 calc R . . . .
 C19 C 0.18706(16) 0.47695(7) 0.64806(12) 0.0361(3) Uani 1 1 d . . . . .
 H19 H 0.1068 0.4907 0.6596 0.043 Uiso 1 1 calc R . . . .
 C20 C 0.31726(16) 0.48728(7) 0.72480(11) 0.0334(3) Uani 1 1 d . . . . .
 H20 H 0.3264 0.5079 0.7892 0.040 Uiso 1 1 calc R . . . .
 C21 C 0.43391(15) 0.46757(7) 0.70772(10) 0.0310(3) Uani 1 1 d . . . . .
 H21 H 0.5233 0.4752 0.7600 0.037 Uiso 1 1 calc R . . . .
 C22 C 0.42065(13) 0.43657(6) 0.61396(10) 0.0263(2) Uani 1 1 d . . . . .
 H22 H 0.5014 0.4231 0.6029 0.032 Uiso 1 1 calc R . . . .
 C23 C 0.20743(12) 0.28969(6) 0.43304(10) 0.0249(2) Uani 1 1 d . . . . .
 C24 C 0.20312(15) 0.23954(7) 0.36409(13) 0.0369(3) Uani 1 1 d . . . . .
 H24 H 0.2254 0.2475 0.3037 0.044 Uiso 1 1 calc R . . . .
 C25 C 0.16644(17) 0.17781(8) 0.38289(16) 0.0481(4) Uani 1 1 d . . . . .
 H25 H 0.1635 0.1441 0.3352 0.058 Uiso 1 1 calc R . . . .
 C26 C 0.13438(17) 0.16570(8) 0.47089(15) 0.0470(4) Uani 1 1 d . . . . .
 H26 H 0.1104 0.1236 0.4840 0.056 Uiso 1 1 calc R . . . .
 C27 C 0.13716(17) 0.21439(8) 0.53929(13) 0.0438(4) Uani 1 1 d . . . . .
 H27 H 0.1141 0.2060 0.5993 0.053 Uiso 1 1 calc R . . . .
 C28 C 0.17380(14) 0.27612(7) 0.52079(11) 0.0321(3) Uani 1 1 d . . . . .
 H28 H 0.1759 0.3095 0.5688 0.038 Uiso 1 1 calc R . . . .
 C29 C 0.11676(12) 0.41664(6) 0.28961(9) 0.0232(2) Uani 1 1 d . . . . .
 C30 C 0.13290(14) 0.48048(7) 0.26660(12) 0.0327(3) Uani 1 1 d . . . . .
 H30 H 0.2114 0.5038 0.3113 0.039 Uiso 1 1 calc R . . . .
 C31 C 0.03576(17) 0.51050(8) 0.17930(14) 0.0431(4) Uani 1 1 d . . . . .
 H31 H 0.0484 0.5540 0.1645 0.052 Uiso 1 1 calc R . . . .
 C32 C -0.07909(17) 0.47732(9) 0.11394(13) 0.0455(4) Uani 1 1 d . . . . .
 H32 H -0.1456 0.4978 0.0543 0.055 Uiso 1 1 calc R . . . .
 C33 C -0.09651(16) 0.41431(9) 0.13585(13) 0.0444(4) Uani 1 1 d . . . . .
 H33 H -0.1754 0.3913 0.0910 0.053 Uiso 1 1 calc R . . . .
 C34 C 0.00056(14) 0.38398(7) 0.22314(11) 0.0320(3) Uani 1 1 d . . . . .
 H34 H -0.0128 0.3405 0.2374 0.038 Uiso 1 1 calc 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 C1 1.9483(11) . ?
 Ge1 C17 1.9463(12) . ?
 Ge1 C23 1.9549(12) . ?
 Ge1 C29 1.9506(12) . ?
 O1 C3 1.2096(15) . ?
 O2 C3 1.3424(15) . ?
 O2 C4 1.4419(15) . ?
 N1 C2 1.4134(15) . ?
 N1 C3 1.3759(15) . ?
 N1 C11 1.4463(15) . ?
 C1 C2 1.3416(16) . ?
 C1 C5 1.4901(16) . ?
 C2 H2 0.9500 . ?
 C4 H4A 0.9800 . ?
 C4 H4B 0.9800 . ?
 C4 H4C 0.9800 . ?
 C5 C6 1.3952(17) . ?
 C5 C10 1.3968(17) . ?
 C6 H6 0.9500 . ?
 C6 C7 1.3853(18) . ?
 C7 H7 0.9500 . ?
 C7 C8 1.385(2) . ?
 C8 H8 0.9500 . ?
 C8 C9 1.379(2) . ?
 C9 H9 0.9500 . ?
 C9 C10 1.3906(18) . ?
 C10 H10 0.9500 . ?
 C11 C12 1.3811(17) . ?
 C11 C16 1.3870(16) . ?
 C12 H12 0.9500 . ?
 C12 C13 1.3894(19) . ?
 C13 H13 0.9500 . ?
 C13 C14 1.380(2) . ?
 C14 H14 0.9500 . ?
 C14 C15 1.380(2) . ?
 C15 H15 0.9500 . ?
 C15 C16 1.3867(18) . ?
 C16 H16 0.9500 . ?
 C17 C18 1.3985(17) . ?
 C17 C22 1.3939(17) . ?
 C18 H18 0.9500 . ?
 C18 C19 1.3892(19) . ?
 C19 H19 0.9500 . ?
 C19 C20 1.384(2) . ?
 C20 H20 0.9500 . ?
 C20 C21 1.381(2) . ?
 C21 H21 0.9500 . ?
 C21 C22 1.3919(18) . ?
 C22 H22 0.9500 . ?
 C23 C24 1.3967(19) . ?
 C23 C28 1.3945(19) . ?
 C24 H24 0.9500 . ?
 C24 C25 1.396(2) . ?
 C25 H25 0.9500 . ?
 C25 C26 1.383(3) . ?
 C26 H26 0.9500 . ?
 C26 C27 1.372(3) . ?
 C27 H27 0.9500 . ?
 C27 C28 1.394(2) . ?
 C28 H28 0.9500 . ?
 C29 C30 1.3946(19) . ?
 C29 C34 1.3886(18) . ?
 C30 H30 0.9500 . ?
 C30 C31 1.389(2) . ?
 C31 H31 0.9500 . ?
 C31 C32 1.380(2) . ?
 C32 H32 0.9500 . ?
 C32 C33 1.377(3) . ?
 C33 H33 0.9500 . ?
 C33 C34 1.392(2) . ?
 C34 H34 0.9500 . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 C1 Ge1 C23 108.15(5) . . ?
 C1 Ge1 C29 106.81(5) . . ?
 C17 Ge1 C1 115.40(5) . . ?
 C17 Ge1 C23 106.81(5) . . ?
 C17 Ge1 C29 108.68(5) . . ?
 C29 Ge1 C23 111.03(5) . . ?
 C3 O2 C4 114.83(10) . . ?
 C2 N1 C11 119.13(9) . . ?
 C3 N1 C2 116.98(10) . . ?
 C3 N1 C11 121.95(10) . . ?
 C2 C1 Ge1 115.30(8) . . ?
 C2 C1 C5 123.99(10) . . ?
 C5 C1 Ge1 120.63(8) . . ?
 N1 C2 H2 116.8 . . ?
 C1 C2 N1 126.39(11) . . ?
 C1 C2 H2 116.8 . . ?
 O1 C3 O2 124.69(11) . . ?
 O1 C3 N1 124.30(11) . . ?
 O2 C3 N1 111.01(10) . . ?
 O2 C4 H4A 109.5 . . ?
 O2 C4 H4B 109.5 . . ?
 O2 C4 H4C 109.5 . . ?
 H4A C4 H4B 109.5 . . ?
 H4A C4 H4C 109.5 . . ?
 H4B C4 H4C 109.5 . . ?
 C6 C5 C1 122.03(11) . . ?
 C6 C5 C10 118.58(11) . . ?
 C10 C5 C1 119.39(11) . . ?
 C5 C6 H6 119.7 . . ?
 C7 C6 C5 120.51(12) . . ?
 C7 C6 H6 119.7 . . ?
 C6 C7 H7 119.8 . . ?
 C8 C7 C6 120.35(13) . . ?
 C8 C7 H7 119.8 . . ?
 C7 C8 H8 120.1 . . ?
 C9 C8 C7 119.78(12) . . ?
 C9 C8 H8 120.1 . . ?
 C8 C9 H9 119.9 . . ?
 C8 C9 C10 120.26(12) . . ?
 C10 C9 H9 119.9 . . ?
 C5 C10 H10 119.8 . . ?
 C9 C10 C5 120.47(12) . . ?
 C9 C10 H10 119.8 . . ?
 C12 C11 N1 119.03(10) . . ?
 C12 C11 C16 120.66(11) . . ?
 C16 C11 N1 120.23(11) . . ?
 C11 C12 H12 120.2 . . ?
 C11 C12 C13 119.58(12) . . ?
 C13 C12 H12 120.2 . . ?
 C12 C13 H13 120.0 . . ?
 C14 C13 C12 120.04(13) . . ?
 C14 C13 H13 120.0 . . ?
 C13 C14 H14 120.0 . . ?
 C13 C14 C15 120.07(13) . . ?
 C15 C14 H14 120.0 . . ?
 C14 C15 H15 119.8 . . ?
 C14 C15 C16 120.44(12) . . ?
 C16 C15 H15 119.8 . . ?
 C11 C16 H16 120.4 . . ?
 C15 C16 C11 119.17(12) . . ?
 C15 C16 H16 120.4 . . ?
 C18 C17 Ge1 118.42(9) . . ?
 C22 C17 Ge1 123.34(9) . . ?
 C22 C17 C18 118.10(11) . . ?
 C17 C18 H18 119.5 . . ?
 C19 C18 C17 121.02(13) . . ?
 C19 C18 H18 119.5 . . ?
 C18 C19 H19 120.0 . . ?
 C20 C19 C18 119.91(13) . . ?
 C20 C19 H19 120.0 . . ?
 C19 C20 H20 120.0 . . ?
 C21 C20 C19 119.99(12) . . ?
 C21 C20 H20 120.0 . . ?
 C20 C21 H21 119.9 . . ?
 C20 C21 C22 120.11(13) . . ?
 C22 C21 H21 119.9 . . ?
 C17 C22 H22 119.6 . . ?
 C21 C22 C17 120.86(12) . . ?
 C21 C22 H22 119.6 . . ?
 C24 C23 Ge1 120.87(11) . . ?
 C28 C23 Ge1 121.18(10) . . ?
 C28 C23 C24 117.94(13) . . ?
 C23 C24 H24 119.6 . . ?
 C25 C24 C23 120.81(16) . . ?
 C25 C24 H24 119.6 . . ?
 C24 C25 H25 120.0 . . ?
 C26 C25 C24 119.96(16) . . ?
 C26 C25 H25 120.0 . . ?
 C25 C26 H26 119.9 . . ?
 C27 C26 C25 120.16(15) . . ?
 C27 C26 H26 119.9 . . ?
 C26 C27 H27 120.0 . . ?
 C26 C27 C28 120.04(16) . . ?
 C28 C27 H27 120.0 . . ?
 C23 C28 H28 119.5 . . ?
 C27 C28 C23 121.08(15) . . ?
 C27 C28 H28 119.5 . . ?
 C30 C29 Ge1 118.88(10) . . ?
 C34 C29 Ge1 122.85(10) . . ?
 C34 C29 C30 118.18(12) . . ?
 C29 C30 H30 119.5 . . ?
 C31 C30 C29 120.93(14) . . ?
 C31 C30 H30 119.5 . . ?
 C30 C31 H31 119.9 . . ?
 C32 C31 C30 120.16(15) . . ?
 C32 C31 H31 119.9 . . ?
 C31 C32 H32 120.2 . . ?
 C33 C32 C31 119.53(14) . . ?
 C33 C32 H32 120.2 . . ?
 C32 C33 H33 119.7 . . ?
 C32 C33 C34 120.55(15) . . ?
 C34 C33 H33 119.7 . . ?
 C29 C34 C33 120.65(14) . . ?
 C29 C34 H34 119.7 . . ?
 C33 C34 H34 119.7 . . ?

_olex2_date_sample_data_collection 2017-07-24
_olex2_date_sample_submission     2017-06-06
_olex2_exptl_crystal_mounting_method cryoloop
_olex2_submission_original_sample_id kd315
_olex2_submission_special_instructions 'No special instructions were received'

################################################################################

data_Compound_23
 
_audit_creation_method            'SHELXL-2017/1'
_shelx_SHELXL_version_number      '2017/1'
_chemical_formula_moiety          'C30 H37 Ge N O3 Si'
_chemical_formula_sum             'C30 H37 Ge N O3 Si'
_chemical_formula_weight          560.28

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0181   0.0091
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0311   0.0180
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0492   0.0322
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Si'  'Si'   0.2541   0.3302
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ge'  'Ge'  -1.0885   0.8855
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/n'
_space_group_name_Hall            '-P 2yn'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, -y-1/2, z-1/2'
 
_cell_length_a                    11.7444(5)
_cell_length_b                    15.9338(8)
_cell_length_c                    32.3292(16)
_cell_angle_alpha                 90
_cell_angle_beta                  92.830(3)
_cell_angle_gamma                 90
_cell_volume                      6042.5(5)
_cell_formula_units_Z             8
_cell_measurement_temperature     200(1)
_cell_measurement_reflns_used     9991
_cell_measurement_theta_min       3.95
_cell_measurement_theta_max       66.32
 
_exptl_crystal_description        'bar'
_exptl_crystal_colour             'colourless'
_exptl_crystal_size_max           0.6
_exptl_crystal_size_mid           0.1
_exptl_crystal_size_min           0.05
_exptl_crystal_density_method     'not measured'
_exptl_crystal_density_diffrn     1.232          
_exptl_crystal_F_000              2352
_exptl_absorpt_coefficient_mu     1.981
_exptl_absorpt_correction_type    numerical 
_exptl_absorpt_correction_T_min   0.528
_exptl_absorpt_correction_T_max   0.899
_exptl_absorpt_process_details     
; 
 SADABS : Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
; 

_diffrn_ambient_temperature       200(1)
_diffrn_radiation_wavelength      1.54178
_diffrn_radiation_type            CuK\a
_diffrn_radiation_source          'micro-source'
_diffrn_measurement_device_type   'Bruker APEX-II CCD'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_reflns_number             47637
_diffrn_reflns_av_unetI/netI      0.0624
_diffrn_reflns_av_R_equivalents   0.0791
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -18
_diffrn_reflns_limit_k_max        18
_diffrn_reflns_limit_l_min        -38
_diffrn_reflns_limit_l_max        38
_diffrn_reflns_theta_min          2.737
_diffrn_reflns_theta_max          66.660
_diffrn_reflns_theta_full         66.500
_diffrn_measured_fraction_theta_max   0.975
_diffrn_measured_fraction_theta_full  0.978
_diffrn_reflns_Laue_measured_fraction_max    0.975
_diffrn_reflns_Laue_measured_fraction_full   0.978
_diffrn_reflns_point_group_measured_fraction_max   0.975
_diffrn_reflns_point_group_measured_fraction_full  0.978
_reflns_number_total              10414
_reflns_number_gt                 8643
_reflns_threshold_expression      'I > 2σ(I)'
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;
 
_computing_data_collection        'Bruker APEX2'
_computing_cell_refinement        'Bruker SAINT'
_computing_data_reduction         'Bruker SAINT'
_computing_structure_solution     'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement   'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics     'SXGRAPH (Farrugia, 2012)'
_computing_publication_material   'WinGX (Farrugia, 2012)'

_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0644P)²+4.1831P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      dual
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_number_reflns          10414
_refine_ls_number_parameters      712
_refine_ls_number_restraints      60
_refine_ls_R_factor_all           0.0558
_refine_ls_R_factor_gt            0.0455
_refine_ls_wR_factor_ref          0.1319
_refine_ls_wR_factor_gt           0.1239
_refine_ls_goodness_of_fit_ref    1.031
_refine_ls_restrained_S_all       1.029
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Ge1 Ge 0.59117(3) 0.18580(2) 0.18081(2) 0.03001(11) Uani 1 1 d . . . . .
Ge2 Ge 0.40896(3) 0.28152(2) 0.39583(2) 0.03059(11) Uani 1 1 d . . . . .
Si2 Si 0.14233(8) 0.17014(6) 0.46475(3) 0.0460(2) Uani 1 1 d . . . . .
O1 O 0.7876(2) 0.28007(14) 0.16219(7) 0.0422(5) Uani 1 1 d . . . . .
O2 O 0.75974(18) -0.02657(16) 0.02737(7) 0.0448(6) Uani 1 1 d . . . . .
O3 O 0.58196(19) -0.02208(18) 0.04919(8) 0.0534(7) Uani 1 1 d . . . . .
O4 O 0.2068(2) 0.24194(13) 0.43738(7) 0.0408(5) Uani 1 1 d . . . . .
O5 O 0.24039(19) 0.65073(14) 0.43938(9) 0.0510(6) Uani 1 1 d . . . . .
O6 O 0.4200(2) 0.61086(16) 0.42920(11) 0.0680(9) Uani 1 1 d . . . . .
N1 N 0.7212(2) 0.06886(17) 0.07532(8) 0.0343(6) Uani 1 1 d . . . . .
N2 N 0.27465(19) 0.51465(15) 0.43093(7) 0.0294(5) Uani 1 1 d . . . . .
C1 C 0.6853(2) 0.1633(2) 0.13333(9) 0.0322(6) Uani 1 1 d . . . . .
C2 C 0.6589(2) 0.09889(19) 0.10849(9) 0.0307(6) Uani 1 1 d . . . . .
H2 H 0.590351 0.069849 0.113653 0.037 Uiso 1 1 calc R U . . .
C3 C 0.8451(3) 0.0741(2) 0.07289(11) 0.0437(8) Uani 1 1 d . . . . .
H3A H 0.884911 0.051891 0.098280 0.052 Uiso 1 1 calc R U . . .
H3B H 0.870101 0.132581 0.068279 0.052 Uiso 1 1 calc R U . . .
C4 C 0.8652(3) 0.0189(2) 0.03553(10) 0.0436(8) Uani 1 1 d . . . . .
H4A H 0.883467 0.053616 0.011337 0.052 Uiso 1 1 calc R U . . .
H4B H 0.929050 -0.020442 0.041693 0.052 Uiso 1 1 calc R U . . .
C5 C 0.6776(3) 0.0048(2) 0.05074(9) 0.0383(7) Uani 1 1 d . . . . .
C6 C 0.7867(3) 0.2211(2) 0.12974(11) 0.0452(8) Uani 1 1 d . . . . .
H6A H 0.858183 0.187984 0.131402 0.054 Uiso 1 1 calc R U . . .
H6B H 0.781582 0.250385 0.102715 0.054 Uiso 1 1 calc R U . . .
C13 C 0.6874(3) 0.16538(19) 0.23086(9) 0.0339(6) Uani 1 1 d . . . . .
C14 C 0.7884(3) 0.1215(3) 0.22855(11) 0.0504(9) Uani 1 1 d . . . . .
H14 H 0.810673 0.102074 0.202363 0.060 Uiso 1 1 calc R U . . .
C15 C 0.8583(4) 0.1052(3) 0.26354(13) 0.0637(11) Uani 1 1 d . . . . .
H15 H 0.927574 0.075237 0.261163 0.076 Uiso 1 1 calc R U . . .
C16 C 0.8267(4) 0.1325(3) 0.30153(13) 0.0623(11) Uani 1 1 d . . . . .
H16 H 0.873788 0.120876 0.325598 0.075 Uiso 1 1 calc R U . . .
C17 C 0.7283(5) 0.1761(3) 0.30475(13) 0.0774(15) Uani 1 1 d . . . . .
H17 H 0.706709 0.195302 0.331056 0.093 Uiso 1 1 calc R U . . .
C18 C 0.6591(4) 0.1926(3) 0.26968(12) 0.0633(11) Uani 1 1 d . . . . .
H18 H 0.590527 0.223272 0.272381 0.076 Uiso 1 1 calc R U . . .
C19 C 0.4640(2) 0.1052(2) 0.18045(9) 0.0331(6) Uani 1 1 d . . . . .
C20 C 0.4822(3) 0.0233(2) 0.19442(10) 0.0440(8) Uani 1 1 d . . . . .
H20 H 0.556790 0.006163 0.203537 0.053 Uiso 1 1 calc R U . . .
C21 C 0.3930(4) -0.0335(3) 0.19518(12) 0.0621(11) Uani 1 1 d . . . . .
H21 H 0.407025 -0.089386 0.204303 0.075 Uiso 1 1 calc R U . . .
C22 C 0.2846(4) -0.0093(3) 0.18282(13) 0.0669(13) Uani 1 1 d . . . . .
H22 H 0.223567 -0.048307 0.183514 0.080 Uiso 1 1 calc R U . . .
C23 C 0.2642(3) 0.0713(3) 0.16943(12) 0.0626(12) Uani 1 1 d . . . . .
H23 H 0.188898 0.088168 0.161078 0.075 Uiso 1 1 calc R U . . .
C24 C 0.3538(3) 0.1286(2) 0.16806(11) 0.0453(8) Uani 1 1 d . . . . .
H24 H 0.339164 0.184157 0.158549 0.054 Uiso 1 1 calc R U . . .
C25 C 0.5206(3) 0.2967(2) 0.17769(11) 0.0415(7) Uani 1 1 d . . . . .
C26 C 0.4602(4) 0.3289(3) 0.20960(13) 0.0687(13) Uani 1 1 d . . . . .
H26 H 0.453787 0.296909 0.234173 0.082 Uiso 1 1 calc R U . . .
C27 C 0.4084(4) 0.4078(4) 0.20643(18) 0.0861(18) Uani 1 1 d . . . . .
H27 H 0.368024 0.429082 0.228915 0.103 Uiso 1 1 calc R U . . .
C28 C 0.4154(4) 0.4538(3) 0.1716(2) 0.0906(18) Uani 1 1 d . . . . .
H28 H 0.380191 0.507446 0.169414 0.109 Uiso 1 1 calc R U . . .
C29 C 0.4729(6) 0.4230(4) 0.1399(3) 0.126(3) Uani 1 1 d . . . . .
H29 H 0.476450 0.454541 0.115063 0.151 Uiso 1 1 calc R U . . .
C30 C 0.5270(5) 0.3455(4) 0.14303(19) 0.093(2) Uani 1 1 d . . . . .
H30 H 0.569420 0.326039 0.120664 0.112 Uiso 1 1 calc R U . . .
C31 C 0.3106(2) 0.36491(18) 0.42038(9) 0.0304(6) Uani 1 1 d . . . . .
C32 C 0.3371(2) 0.44559(18) 0.41743(8) 0.0275(6) Uani 1 1 d . . . . .
H32 H 0.406364 0.458038 0.404725 0.033 Uiso 1 1 calc R U . . .
C33 C 0.1511(2) 0.5183(2) 0.43310(10) 0.0339(6) Uani 1 1 d . . . . .
H33A H 0.124038 0.480127 0.454705 0.041 Uiso 1 1 calc R U . . .
H33B H 0.112282 0.503948 0.406140 0.041 Uiso 1 1 calc R U . . .
C34 C 0.1324(3) 0.6098(2) 0.44431(11) 0.0404(7) Uani 1 1 d . . . . .
H34A H 0.072404 0.635095 0.425681 0.048 Uiso 1 1 calc R U . . .
H34B H 0.109253 0.614808 0.473242 0.048 Uiso 1 1 calc R U . . .
C35 C 0.3214(3) 0.5931(2) 0.43299(12) 0.0423(8) Uani 1 1 d . . . . .
C36 C 0.2084(3) 0.3301(2) 0.44200(11) 0.0435(8) Uani 1 1 d . . . . .
H36A H 0.214192 0.345052 0.471757 0.052 Uiso 1 1 calc R U . . .
H36B H 0.137132 0.354547 0.429607 0.052 Uiso 1 1 calc R U . . .
C37 C 0.2032(4) 0.0701(3) 0.4459(2) 0.100(2) Uani 1 1 d . . . . .
H37A H 0.169994 0.022710 0.460380 0.150 Uiso 1 1 calc R U . . .
H37B H 0.185637 0.064578 0.416025 0.150 Uiso 1 1 calc R U . . .
H37C H 0.286093 0.070257 0.451204 0.150 Uiso 1 1 calc R U . . .
C38 C 0.1808(6) 0.1863(5) 0.52065(15) 0.120(3) Uani 1 1 d . . . . .
H38A H 0.142754 0.143817 0.536996 0.180 Uiso 1 1 calc R U . . .
H38B H 0.263601 0.181163 0.525416 0.180 Uiso 1 1 calc R U . . .
H38C H 0.156459 0.242333 0.528992 0.180 Uiso 1 1 calc R U . . .
C39 C -0.0170(3) 0.1732(2) 0.45459(11) 0.0442(8) Uani 1 1 d . . . . .
C40 C -0.0455(5) 0.1791(5) 0.40784(17) 0.099(2) Uani 1 1 d . . . . .
H40A H -0.010497 0.229731 0.396826 0.149 Uiso 1 1 calc R U . . .
H40B H -0.015932 0.129524 0.394033 0.149 Uiso 1 1 calc R U . . .
H40C H -0.128427 0.181970 0.402796 0.149 Uiso 1 1 calc R U . . .
C41 C -0.0692(5) 0.2498(3) 0.4745(2) 0.0887(17) Uani 1 1 d . . . . .
H41A H -0.035359 0.300879 0.463593 0.133 Uiso 1 1 calc R U . . .
H41B H -0.151725 0.250282 0.468279 0.133 Uiso 1 1 calc R U . . .
H41C H -0.054197 0.247468 0.504615 0.133 Uiso 1 1 calc R U . . .
C42 C -0.0710(4) 0.0947(4) 0.4721(2) 0.100(2) Uani 1 1 d . . . . .
H42A H -0.038318 0.044807 0.459576 0.150 Uiso 1 1 calc R U . . .
H42B H -0.055978 0.093081 0.502192 0.150 Uiso 1 1 calc R U . . .
H42C H -0.153505 0.095895 0.465856 0.150 Uiso 1 1 calc R U . . .
C43 C 0.4781(3) 0.2104(2) 0.43938(10) 0.0355(7) Uani 1 1 d . . . . .
C44 C 0.5067(3) 0.2460(2) 0.47783(11) 0.0483(8) Uani 1 1 d . . . . .
H44 H 0.486966 0.302754 0.482802 0.058 Uiso 1 1 calc R U . . .
C45 C 0.5637(4) 0.2002(3) 0.50912(12) 0.0570(10) Uani 1 1 d . . . . .
H45 H 0.583463 0.225934 0.534989 0.068 Uiso 1 1 calc R U . . .
C46 C 0.5911(3) 0.1175(3) 0.50248(12) 0.0562(10) Uani 1 1 d . . . . .
H46 H 0.629130 0.085709 0.523840 0.067 Uiso 1 1 calc R U . . .
C47 C 0.5633(4) 0.0811(2) 0.46465(13) 0.0571(10) Uani 1 1 d . . . . .
H47 H 0.582624 0.024075 0.460035 0.068 Uiso 1 1 calc R U . . .
C48 C 0.5071(3) 0.1269(2) 0.43311(11) 0.0448(8) Uani 1 1 d . . . . .
H48 H 0.488524 0.100970 0.407186 0.054 Uiso 1 1 calc R U . . .
C49 C 0.5370(3) 0.33944(19) 0.37097(10) 0.0343(6) Uani 1 1 d . . . . .
C50 C 0.6451(3) 0.3427(2) 0.39108(12) 0.0463(8) Uani 1 1 d . . . . .
H50 H 0.656578 0.319357 0.418006 0.056 Uiso 1 1 calc R U . . .
C51 C 0.7359(3) 0.3798(3) 0.37203(15) 0.0618(11) Uani 1 1 d . . . . .
H51 H 0.809080 0.381429 0.385916 0.074 Uiso 1 1 calc R U . . .
C52 C 0.7202(4) 0.4143(3) 0.33309(15) 0.0688(13) Uani 1 1 d . . . . .
H52 H 0.782445 0.439535 0.320096 0.083 Uiso 1 1 calc R U . . .
C53 C 0.6144(4) 0.4121(3) 0.31312(13) 0.0625(11) Uani 1 1 d . . . . .
H53 H 0.603268 0.436563 0.286427 0.075 Uiso 1 1 calc R U . . .
C54 C 0.5236(3) 0.3745(2) 0.33166(11) 0.0457(8) Uani 1 1 d . . . . .
H54 H 0.451160 0.372545 0.317283 0.055 Uiso 1 1 calc R U . . .
C55 C 0.3269(3) 0.22474(19) 0.34941(9) 0.0363(7) Uani 1 1 d . . . . .
C56 C 0.3843(3) 0.1724(2) 0.32292(11) 0.0486(8) Uani 1 1 d . . . . .
H56 H 0.462729 0.160423 0.328627 0.058 Uiso 1 1 calc R U . . .
C57 C 0.3275(4) 0.1373(2) 0.28791(11) 0.0603(11) Uani 1 1 d . . . . .
H57 H 0.367469 0.101203 0.270252 0.072 Uiso 1 1 calc R U . . .
C58 C 0.2152(4) 0.1545(3) 0.27909(12) 0.0612(11) Uani 1 1 d . . . . .
H58 H 0.177295 0.130709 0.255253 0.073 Uiso 1 1 calc R U . . .
C59 C 0.1566(4) 0.2065(3) 0.30467(12) 0.0597(10) Uani 1 1 d . . . . .
H59 H 0.078441 0.218851 0.298456 0.072 Uiso 1 1 calc R U . . .
C60 C 0.2126(3) 0.2409(2) 0.33968(11) 0.0465(8) Uani 1 1 d . . . . .
H60 H 0.171574 0.276270 0.357326 0.056 Uiso 1 1 calc R U . . .
Si1A Si 0.85754(9) 0.37045(7) 0.16685(3) 0.0388(2) Uani 0.85 1 d D . P A 1
C7A C 0.8154(5) 0.4102(4) 0.21786(16) 0.0685(14) Uani 0.85 1 d D . P A 1
H7A H 0.852730 0.464245 0.223656 0.103 Uiso 0.85 1 calc R U P A 1
H7B H 0.732495 0.417542 0.217330 0.103 Uiso 0.85 1 calc R U P A 1
H7C H 0.838744 0.369840 0.239521 0.103 Uiso 0.85 1 calc R U P A 1
C8A C 0.8096(6) 0.4442(4) 0.1247(2) 0.0797(19) Uani 0.85 1 d D . P A 1
H8A H 0.851552 0.497152 0.127887 0.120 Uiso 0.85 1 calc R U P A 1
H8B H 0.824155 0.419252 0.097774 0.120 Uiso 0.85 1 calc R U P A 1
H8C H 0.727737 0.454993 0.126314 0.120 Uiso 0.85 1 calc R U P A 1
C9A C 1.0161(4) 0.3527(3) 0.16600(15) 0.0527(11) Uani 0.85 1 d D . P A 1
C10A C 1.0531(6) 0.2850(5) 0.1969(3) 0.097(3) Uani 0.85 1 d D . P A 1
H10A H 1.029441 0.300699 0.224503 0.145 Uiso 0.85 1 calc R U P A 1
H10B H 1.017634 0.231558 0.188644 0.145 Uiso 0.85 1 calc R U P A 1
H10C H 1.136280 0.279216 0.197514 0.145 Uiso 0.85 1 calc R U P A 1
C11A C 1.0537(6) 0.3273(5) 0.1229(2) 0.094(3) Uani 0.85 1 d D . P A 1
H11A H 1.030140 0.370654 0.102772 0.141 Uiso 0.85 1 calc R U P A 1
H11B H 1.136868 0.321411 0.123707 0.141 Uiso 0.85 1 calc R U P A 1
H11C H 1.018221 0.273753 0.114837 0.141 Uiso 0.85 1 calc R U P A 1
C12A C 1.0772(6) 0.4354(6) 0.1783(3) 0.082(2) Uani 0.85 1 d D . P A 1
H12A H 1.053881 0.479538 0.158522 0.123 Uiso 0.85 1 calc R U P A 1
H12B H 1.056677 0.451925 0.206155 0.123 Uiso 0.85 1 calc R U P A 1
H12C H 1.159889 0.427321 0.177991 0.123 Uiso 0.85 1 calc R U P A 1
Si1B Si 0.9140(7) 0.3154(5) 0.1849(2) 0.0558(17) Uani 0.15 1 d D . P A 2
C7B C 0.874(3) 0.354(2) 0.2367(8) 0.103(13) Uani 0.15 1 d D . P A 2
H7D H 0.941803 0.375141 0.252015 0.154 Uiso 0.15 1 calc R U P A 2
H7E H 0.817255 0.398441 0.233157 0.154 Uiso 0.15 1 calc R U P A 2
H7F H 0.841627 0.307071 0.252148 0.154 Uiso 0.15 1 calc R U P A 2
C8B C 1.036(2) 0.2393(19) 0.1896(10) 0.072(8) Uani 0.15 1 d D . P A 2
H8D H 1.102178 0.266924 0.202959 0.107 Uiso 0.15 1 calc R U P A 2
H8E H 1.013731 0.191110 0.206302 0.107 Uiso 0.15 1 calc R U P A 2
H8F H 1.054198 0.219985 0.161948 0.107 Uiso 0.15 1 calc R U P A 2
C9B C 0.960(3) 0.4062(13) 0.1529(7) 0.085(8) Uani 0.15 1 d D . P A 2
C10B C 0.995(4) 0.376(2) 0.1110(10) 0.108(15) Uani 0.15 1 d D . P A 2
H10D H 0.930632 0.346711 0.096727 0.161 Uiso 0.15 1 calc R U P A 2
H10E H 1.017793 0.423560 0.094334 0.161 Uiso 0.15 1 calc R U P A 2
H10F H 1.059238 0.336631 0.114791 0.161 Uiso 0.15 1 calc R U P A 2
C11B C 0.860(4) 0.470(3) 0.1478(19) 0.18(3) Uani 0.15 1 d D . P A 2
H11D H 0.838712 0.488555 0.175182 0.273 Uiso 0.15 1 calc R U P A 2
H11E H 0.884119 0.517789 0.131597 0.273 Uiso 0.15 1 calc R U P A 2
H11F H 0.794685 0.442270 0.133468 0.273 Uiso 0.15 1 calc R U P A 2
C12B C 1.061(5) 0.452(4) 0.1756(18) 0.15(3) Uani 0.15 1 d D . P A 2
H12D H 1.037432 0.471399 0.202644 0.224 Uiso 0.15 1 calc R U P A 2
H12E H 1.125036 0.412952 0.179513 0.224 Uiso 0.15 1 calc R U P A 2
H12F H 1.083591 0.499882 0.159056 0.224 Uiso 0.15 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
Ge1 C25 1.953(3) . ?
Ge1 C13 1.955(3) . ?
Ge1 C1 1.968(3) . ?
Ge1 C19 1.970(3) . ?
Ge2 C43 1.953(3) . ?
Ge2 C31 1.955(3) . ?
Ge2 C55 1.964(3) . ?
Ge2 C49 1.969(3) . ?
Si2 O4 1.653(2) . ?
Si2 C38 1.859(5) . ?
Si2 C37 1.863(5) . ?
Si2 C39 1.885(4) . ?
O1 C6 1.408(4) . ?
O1 Si1A 1.661(2) . ?
O1 Si1B 1.718(7) . ?
O2 C5 1.350(4) . ?
O2 C4 1.448(4) . ?
O3 C5 1.201(4) . ?
O4 C36 1.413(4) . ?
O5 C35 1.346(4) . ?
O5 C34 1.442(4) . ?
O6 C35 1.204(4) . ?
N1 C5 1.377(4) . ?
N1 C2 1.411(4) . ?
N1 C3 1.464(4) . ?
N2 C35 1.365(4) . ?
N2 C32 1.404(4) . ?
N2 C33 1.457(3) . ?
C1 C2 1.330(4) . ?
C1 C6 1.515(4) . ?
C3 C4 1.522(4) . ?
C13 C14 1.382(5) . ?
C13 C18 1.384(5) . ?
C14 C15 1.389(5) . ?
C15 C16 1.371(6) . ?
C16 C17 1.357(7) . ?
C17 C18 1.387(6) . ?
C19 C24 1.387(5) . ?
C19 C20 1.394(5) . ?
C20 C21 1.385(5) . ?
C21 C22 1.371(7) . ?
C22 C23 1.373(7) . ?
C23 C24 1.395(6) . ?
C25 C30 1.369(6) . ?
C25 C26 1.379(5) . ?
C26 C27 1.398(6) . ?
C27 C28 1.351(8) . ?
C28 C29 1.347(9) . ?
C29 C30 1.389(7) . ?
C31 C32 1.327(4) . ?
C31 C36 1.522(4) . ?
C33 C34 1.522(4) . ?
C39 C42 1.523(6) . ?
C39 C41 1.524(6) . ?
C39 C40 1.535(6) . ?
C43 C48 1.390(5) . ?
C43 C44 1.392(5) . ?
C44 C45 1.391(5) . ?
C45 C46 1.376(6) . ?
C46 C47 1.378(6) . ?
C47 C48 1.394(5) . ?
C49 C54 1.390(5) . ?
C49 C50 1.399(5) . ?
C50 C51 1.390(5) . ?
C51 C52 1.378(7) . ?
C52 C53 1.373(7) . ?
C53 C54 1.384(5) . ?
C55 C60 1.388(5) . ?
C55 C56 1.393(5) . ?
C56 C57 1.402(5) . ?
C57 C58 1.364(6) . ?
C58 C59 1.379(6) . ?
C59 C60 1.393(5) . ?
Si1A C7A 1.857(5) . ?
Si1A C8A 1.865(6) . ?
Si1A C9A 1.885(5) . ?
C9A C10A 1.518(9) . ?
C9A C11A 1.535(7) . ?
C9A C12A 1.544(7) . ?
Si1B C7B 1.863(16) . ?
Si1B C9B 1.872(16) . ?
Si1B C8B 1.873(18) . ?
C9B C10B 1.52(2) . ?
C9B C12B 1.544(19) . ?
C9B C11B 1.55(2) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
C25 Ge1 C13 114.85(14) . . ?
C25 Ge1 C1 112.21(14) . . ?
C13 Ge1 C1 106.93(13) . . ?
C25 Ge1 C19 105.66(13) . . ?
C13 Ge1 C19 107.68(13) . . ?
C1 Ge1 C19 109.35(12) . . ?
C43 Ge2 C31 109.55(13) . . ?
C43 Ge2 C55 117.02(13) . . ?
C31 Ge2 C55 110.25(13) . . ?
C43 Ge2 C49 105.53(13) . . ?
C31 Ge2 C49 109.01(12) . . ?
C55 Ge2 C49 105.06(13) . . ?
O4 Si2 C38 109.2(2) . . ?
O4 Si2 C37 102.90(19) . . ?
C38 Si2 C37 111.0(4) . . ?
O4 Si2 C39 111.49(15) . . ?
C38 Si2 C39 111.0(2) . . ?
C37 Si2 C39 111.0(2) . . ?
C6 O1 Si1A 129.2(2) . . ?
C6 O1 Si1B 120.8(3) . . ?
C5 O2 C4 110.0(2) . . ?
C36 O4 Si2 129.5(2) . . ?
C35 O5 C34 109.9(2) . . ?
C5 N1 C2 119.9(2) . . ?
C5 N1 C3 110.7(2) . . ?
C2 N1 C3 125.1(2) . . ?
C35 N2 C32 121.2(2) . . ?
C35 N2 C33 111.1(2) . . ?
C32 N2 C33 125.6(2) . . ?
C2 C1 C6 125.7(3) . . ?
C2 C1 Ge1 119.2(2) . . ?
C6 C1 Ge1 115.0(2) . . ?
C1 C2 N1 127.3(3) . . ?
N1 C3 C4 101.7(2) . . ?
O2 C4 C3 105.6(2) . . ?
O3 C5 O2 122.5(3) . . ?
O3 C5 N1 127.5(3) . . ?
O2 C5 N1 110.0(3) . . ?
O1 C6 C1 109.0(3) . . ?
C14 C13 C18 116.9(3) . . ?
C14 C13 Ge1 120.2(2) . . ?
C18 C13 Ge1 122.9(3) . . ?
C13 C14 C15 121.6(3) . . ?
C16 C15 C14 119.7(4) . . ?
C17 C16 C15 120.0(4) . . ?
C16 C17 C18 120.1(4) . . ?
C13 C18 C17 121.7(4) . . ?
C24 C19 C20 118.2(3) . . ?
C24 C19 Ge1 121.5(3) . . ?
C20 C19 Ge1 120.3(2) . . ?
C21 C20 C19 120.8(4) . . ?
C22 C21 C20 120.2(4) . . ?
C21 C22 C23 120.0(4) . . ?
C22 C23 C24 120.1(4) . . ?
C19 C24 C23 120.6(4) . . ?
C30 C25 C26 116.9(4) . . ?
C30 C25 Ge1 121.1(3) . . ?
C26 C25 Ge1 122.0(3) . . ?
C25 C26 C27 121.2(5) . . ?
C28 C27 C26 120.4(5) . . ?
C29 C28 C27 119.3(5) . . ?
C28 C29 C30 120.9(6) . . ?
C25 C30 C29 121.4(5) . . ?
C32 C31 C36 125.3(3) . . ?
C32 C31 Ge2 118.9(2) . . ?
C36 C31 Ge2 115.7(2) . . ?
C31 C32 N2 127.5(3) . . ?
N2 C33 C34 101.8(2) . . ?
O5 C34 C33 105.6(2) . . ?
O6 C35 O5 123.0(3) . . ?
O6 C35 N2 126.6(3) . . ?
O5 C35 N2 110.3(3) . . ?
O4 C36 C31 108.7(2) . . ?
C42 C39 C41 108.4(4) . . ?
C42 C39 C40 110.0(4) . . ?
C41 C39 C40 107.1(4) . . ?
C42 C39 Si2 110.0(3) . . ?
C41 C39 Si2 111.3(3) . . ?
C40 C39 Si2 109.9(3) . . ?
C48 C43 C44 118.0(3) . . ?
C48 C43 Ge2 123.1(2) . . ?
C44 C43 Ge2 118.7(2) . . ?
C45 C44 C43 121.5(3) . . ?
C46 C45 C44 119.8(4) . . ?
C45 C46 C47 119.6(3) . . ?
C46 C47 C48 120.8(4) . . ?
C43 C48 C47 120.3(3) . . ?
C54 C49 C50 118.0(3) . . ?
C54 C49 Ge2 120.5(3) . . ?
C50 C49 Ge2 121.4(3) . . ?
C51 C50 C49 120.6(4) . . ?
C52 C51 C50 120.3(4) . . ?
C53 C52 C51 119.8(4) . . ?
C52 C53 C54 120.4(4) . . ?
C53 C54 C49 121.0(4) . . ?
C60 C55 C56 117.6(3) . . ?
C60 C55 Ge2 121.4(2) . . ?
C56 C55 Ge2 120.8(3) . . ?
C55 C56 C57 120.7(4) . . ?
C58 C57 C56 120.3(4) . . ?
C57 C58 C59 120.2(4) . . ?
C58 C59 C60 119.6(4) . . ?
C55 C60 C59 121.6(3) . . ?
O1 Si1A C7A 103.0(2) . . ?
O1 Si1A C8A 110.5(2) . . ?
C7A Si1A C8A 110.5(3) . . ?
O1 Si1A C9A 110.65(17) . . ?
C7A Si1A C9A 111.8(2) . . ?
C8A Si1A C9A 110.3(3) . . ?
C10A C9A C11A 108.9(6) . . ?
C10A C9A C12A 108.8(6) . . ?
C11A C9A C12A 107.9(5) . . ?
C10A C9A Si1A 110.4(4) . . ?
C11A C9A Si1A 112.4(4) . . ?
C12A C9A Si1A 108.4(4) . . ?
O1 Si1B C7B 103.9(13) . . ?
O1 Si1B C9B 106.4(10) . . ?
C7B Si1B C9B 109.7(13) . . ?
O1 Si1B C8B 117.4(12) . . ?
C7B Si1B C8B 111.3(15) . . ?
C9B Si1B C8B 107.8(13) . . ?
C10B C9B C12B 110(2) . . ?
C10B C9B C11B 111(2) . . ?
C12B C9B C11B 108(2) . . ?
C10B C9B Si1B 110.1(17) . . ?
C12B C9B Si1B 110(2) . . ?
C11B C9B Si1B 109.0(19) . . ?
 
_refine_diff_density_max    0.367
_refine_diff_density_min   -0.399
_refine_diff_density_rms    0.076



################################################################################

data_Compound_25
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_formula_moiety          'C26 H24 F3 Ge N O2'
_chemical_formula_sum             'C26 H24 F3 Ge N O2'
_chemical_formula_weight          512.05

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'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'F'  'F'   0.0171   0.0103
 '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                    11.4162(3)
_cell_length_b                    16.8675(5)
_cell_length_c                    24.7995(7)
_cell_angle_alpha                 90
_cell_angle_beta                  96.907(2)
_cell_angle_gamma                 90
_cell_volume                      4740.8(2)
_cell_formula_units_Z             8
_cell_measurement_temperature     200(1)
_cell_measurement_reflns_used     9923
_cell_measurement_theta_min       2.24
_cell_measurement_theta_max       30.35
 
_exptl_crystal_description        'fragment'
_exptl_crystal_colour             'colourless'
_exptl_crystal_size_max           0.35
_exptl_crystal_size_mid           0.15
_exptl_crystal_size_min           0.05
_exptl_crystal_density_method     'not measured'
_exptl_crystal_density_diffrn     1.435          
_exptl_crystal_F_000              2096
_exptl_absorpt_coefficient_mu     1.339
_exptl_absorpt_correction_type    numerical 
_exptl_absorpt_correction_T_min   0.802
_exptl_absorpt_correction_T_max   0.953
_exptl_absorpt_process_details     
; 
 SADABS : Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
; 
 
_diffrn_ambient_temperature       200(1)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   'curved graphite'
_diffrn_measurement_device_type   'Bruker APEX-II CCD'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_reflns_number             61522
_diffrn_reflns_av_unetI/netI      0.0337
_diffrn_reflns_av_R_equivalents   0.0319
_diffrn_reflns_limit_h_min        -15
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        -24
_diffrn_reflns_limit_k_max        24
_diffrn_reflns_limit_l_min        -30
_diffrn_reflns_limit_l_max        35
_diffrn_reflns_theta_min          2.048
_diffrn_reflns_theta_max          30.569
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.998
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    0.998
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   0.998
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              14521
_reflns_number_gt                 10801
_reflns_threshold_expression      'I > 2σ(I)'
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;
 
_computing_data_collection        'Bruker APEX2'
_computing_cell_refinement        'Bruker SAINT'
_computing_data_reduction         'Bruker SAINT'
_computing_structure_solution     'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement   'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics     'SXGRAPH (Farrugia, 2012)'
_computing_publication_material   'WinGX (Farrugia, 2012)'

_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0362P)²+1.3268P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      dual
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_number_reflns          14521
_refine_ls_number_parameters      595
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0561
_refine_ls_R_factor_gt            0.0333
_refine_ls_wR_factor_ref          0.0787
_refine_ls_wR_factor_gt           0.0716
_refine_ls_goodness_of_fit_ref    1.006
_refine_ls_restrained_S_all       1.006
_refine_ls_shift/su_max           0.002
_refine_ls_shift/su_mean          0.000
_refine_diff_density_max          0.464
_refine_diff_density_min         -0.348
_refine_diff_density_rms          0.058
 
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 0.04864(2) 0.63226(2) 0.13830(2) 0.02170(4) Uani 1 1 d . . . . .
Ge2 Ge 0.47576(2) 0.60589(2) 0.38377(2) 0.02348(4) Uani 1 1 d . . . . .
F1 F 0.14550(15) 0.66166(8) 0.26972(5) 0.0712(4) Uani 1 1 d . . . . .
F2 F 0.06495(14) 0.56185(7) 0.30100(5) 0.0632(4) Uani 1 1 d . . . . .
F3 F -0.03989(14) 0.64991(10) 0.25602(6) 0.0788(5) Uani 1 1 d . . . . .
F4 F 0.47626(12) 0.67089(7) 0.22082(4) 0.0517(3) Uani 1 1 d . . . . .
F5 F 0.38991(12) 0.57068(7) 0.25062(5) 0.0547(3) Uani 1 1 d . . . . .
F6 F 0.57622(11) 0.58395(8) 0.27025(5) 0.0572(3) Uani 1 1 d . . . . .
O1 O 0.05772(10) 0.37198(7) 0.09072(5) 0.0318(3) Uani 1 1 d . . . . .
O2 O -0.06023(10) 0.47047(7) 0.11241(5) 0.0315(3) Uani 1 1 d . . . . .
O3 O 0.44268(10) 0.87349(7) 0.42145(5) 0.0322(3) Uani 1 1 d . . . . .
O4 O 0.57109(10) 0.77647(7) 0.40797(5) 0.0303(3) Uani 1 1 d . . . . .
N1 N 0.11290(11) 0.43947(7) 0.16641(5) 0.0224(3) Uani 1 1 d . . . . .
N2 N 0.40139(11) 0.79796(7) 0.34847(5) 0.0223(3) Uani 1 1 d . . . . .
C1 C 0.06817(13) 0.56740(9) 0.20509(6) 0.0234(3) Uani 1 1 d . . . . .
C2 C 0.05981(18) 0.60853(10) 0.25743(7) 0.0365(4) Uani 1 1 d . . . . .
C3 C 0.10365(13) 0.49169(9) 0.20918(7) 0.0246(3) Uani 1 1 d . . . . .
H3 H 0.1246 0.4716 0.2448 0.030 Uiso 1 1 calc R U . . .
C4 C 0.02843(13) 0.43210(9) 0.12222(7) 0.0245(3) Uani 1 1 d . . . . .
C5 C 0.17629(15) 0.34635(11) 0.11078(7) 0.0325(4) Uani 1 1 d . . . . .
H5A H 0.2354 0.3736 0.0912 0.039 Uiso 1 1 calc R U . . .
H5B H 0.1848 0.2884 0.1064 0.039 Uiso 1 1 calc R U . . .
C6 C 0.19137(13) 0.36936(9) 0.17103(7) 0.0253(3) Uani 1 1 d . . . . .
C7 C 0.31778(14) 0.39117(11) 0.19135(8) 0.0346(4) Uani 1 1 d . . . . .
H7A H 0.3667 0.3433 0.1938 0.052 Uiso 1 1 calc R U . . .
H7B H 0.3475 0.4287 0.1660 0.052 Uiso 1 1 calc R U . . .
H7C H 0.3208 0.4157 0.2273 0.052 Uiso 1 1 calc R U . . .
C8 C 0.14422(17) 0.30593(11) 0.20613(8) 0.0394(4) Uani 1 1 d . . . . .
H8A H 0.1974 0.2601 0.2087 0.059 Uiso 1 1 calc R U . . .
H8B H 0.1394 0.3272 0.2426 0.059 Uiso 1 1 calc R U . . .
H8C H 0.0655 0.2895 0.1898 0.059 Uiso 1 1 calc R U . . .
C9 C 0.09892(14) 0.74168(9) 0.15491(6) 0.0261(3) Uani 1 1 d . . . . .
C10 C 0.01459(18) 0.79795(11) 0.16406(9) 0.0417(4) Uani 1 1 d . . . . .
H10 H -0.0643 0.7816 0.1664 0.050 Uiso 1 1 calc R U . . .
C11 C 0.0436(2) 0.87788(12) 0.16991(10) 0.0525(6) Uani 1 1 d . . . . .
H11 H -0.0150 0.9153 0.1767 0.063 Uiso 1 1 calc R U . . .
C12 C 0.1571(2) 0.90278(12) 0.16589(9) 0.0524(6) Uani 1 1 d . . . . .
H12 H 0.1766 0.9575 0.1689 0.063 Uiso 1 1 calc R U . . .
C13 C 0.2416(2) 0.84793(13) 0.15757(10) 0.0533(6) Uani 1 1 d . . . . .
H13 H 0.3204 0.8646 0.1554 0.064 Uiso 1 1 calc R U . . .
C14 C 0.21285(17) 0.76801(11) 0.15234(8) 0.0394(4) Uani 1 1 d . . . . .
H14 H 0.2727 0.7307 0.1469 0.047 Uiso 1 1 calc R U . . .
C15 C 0.15690(13) 0.58696(9) 0.09188(6) 0.0229(3) Uani 1 1 d . . . . .
C16 C 0.27536(14) 0.57741(10) 0.11281(7) 0.0274(3) Uani 1 1 d . . . . .
H16 H 0.3011 0.5946 0.1488 0.033 Uiso 1 1 calc R U . . .
C17 C 0.35570(14) 0.54350(11) 0.08230(8) 0.0335(4) Uani 1 1 d . . . . .
H17 H 0.4360 0.5382 0.0971 0.040 Uiso 1 1 calc R U . . .
C18 C 0.31916(16) 0.51739(11) 0.03023(7) 0.0362(4) Uani 1 1 d . . . . .
H18 H 0.3741 0.4936 0.0093 0.043 Uiso 1 1 calc R U . . .
C19 C 0.20272(16) 0.52600(11) 0.00871(7) 0.0349(4) Uani 1 1 d . . . . .
H19 H 0.1774 0.5078 -0.0271 0.042 Uiso 1 1 calc R U . . .
C20 C 0.12224(14) 0.56114(10) 0.03906(7) 0.0277(3) Uani 1 1 d . . . . .
H20 H 0.0426 0.5676 0.0236 0.033 Uiso 1 1 calc R U . . .
C21 C -0.11414(14) 0.64262(9) 0.10545(7) 0.0290(3) Uani 1 1 d . . . . .
C22 C -0.20828(15) 0.61608(10) 0.13133(9) 0.0396(5) Uani 1 1 d . . . . .
H22 H -0.1932 0.5903 0.1655 0.048 Uiso 1 1 calc R U . . .
C23 C -0.32394(17) 0.62665(12) 0.10805(12) 0.0553(6) Uani 1 1 d . . . . .
H23 H -0.3872 0.6088 0.1265 0.066 Uiso 1 1 calc R U . . .
C24 C -0.34705(19) 0.66289(14) 0.05835(11) 0.0603(7) Uani 1 1 d . . . . .
H24 H -0.4262 0.6690 0.0420 0.072 Uiso 1 1 calc R U . . .
C25 C -0.2555(2) 0.69040(15) 0.03218(9) 0.0601(7) Uani 1 1 d . . . . .
H25 H -0.2717 0.7157 -0.0021 0.072 Uiso 1 1 calc R U . . .
C26 C -0.13891(18) 0.68137(13) 0.05581(8) 0.0446(5) Uani 1 1 d . . . . .
H26 H -0.0763 0.7018 0.0379 0.053 Uiso 1 1 calc R U . . .
C27 C 0.45681(13) 0.66808(9) 0.31576(6) 0.0239(3) Uani 1 1 d . . . . .
C28 C 0.47443(17) 0.62474(10) 0.26485(7) 0.0348(4) Uani 1 1 d . . . . .
C29 C 0.41887(13) 0.74283(9) 0.30864(6) 0.0233(3) Uani 1 1 d . . . . .
H29 H 0.4019 0.7602 0.2721 0.028 Uiso 1 1 calc R U . . .
C30 C 0.48041(13) 0.81135(9) 0.39403(7) 0.0251(3) Uani 1 1 d . . . . .
C31 C 0.32519(15) 0.89529(10) 0.39694(7) 0.0317(4) Uani 1 1 d . . . . .
H31A H 0.3140 0.9534 0.3980 0.038 Uiso 1 1 calc R U . . .
H31B H 0.2642 0.8694 0.4161 0.038 Uiso 1 1 calc R U . . .
C32 C 0.31875(13) 0.86579(9) 0.33830(7) 0.0254(3) Uani 1 1 d . . . . .
C33 C 0.36599(15) 0.92726(10) 0.30134(8) 0.0336(4) Uani 1 1 d . . . . .
H33A H 0.3098 0.9712 0.2953 0.050 Uiso 1 1 calc R U . . .
H33B H 0.4420 0.9474 0.3185 0.050 Uiso 1 1 calc R U . . .
H33C H 0.3765 0.9027 0.2664 0.050 Uiso 1 1 calc R U . . .
C34 C 0.19550(14) 0.83821(11) 0.31550(8) 0.0328(4) Uani 1 1 d . . . . .
H34A H 0.1433 0.8843 0.3093 0.049 Uiso 1 1 calc R U . . .
H34B H 0.1994 0.8103 0.2811 0.049 Uiso 1 1 calc R U . . .
H34C H 0.1646 0.8023 0.3415 0.049 Uiso 1 1 calc R U . . .
C35 C 0.38461(15) 0.65550(10) 0.43582(7) 0.0279(3) Uani 1 1 d . . . . .
C36 C 0.26626(16) 0.67422(11) 0.42066(8) 0.0355(4) Uani 1 1 d . . . . .
H36 H 0.2311 0.6626 0.3849 0.043 Uiso 1 1 calc R U . . .
C37 C 0.19929(19) 0.70944(14) 0.45705(9) 0.0499(5) Uani 1 1 d . . . . .
H37 H 0.1189 0.7222 0.4460 0.060 Uiso 1 1 calc R U . . .
C38 C 0.2494(2) 0.72607(14) 0.50935(9) 0.0549(6) Uani 1 1 d . . . . .
H38 H 0.2038 0.7506 0.5343 0.066 Uiso 1 1 calc R U . . .
C39 C 0.3659(2) 0.70684(14) 0.52511(9) 0.0521(6) Uani 1 1 d . . . . .
H39 H 0.4001 0.7174 0.5612 0.062 Uiso 1 1 calc R U . . .
C40 C 0.43333(17) 0.67223(11) 0.48870(8) 0.0377(4) Uani 1 1 d . . . . .
H40 H 0.5137 0.6598 0.5000 0.045 Uiso 1 1 calc R U . . .
C41 C 0.64178(14) 0.58869(10) 0.40912(7) 0.0293(3) Uani 1 1 d . . . . .
C42 C 0.73129(15) 0.62912(11) 0.38769(8) 0.0373(4) Uani 1 1 d . . . . .
H42 H 0.7115 0.6689 0.3610 0.045 Uiso 1 1 calc R U . . .
C43 C 0.84913(17) 0.61270(13) 0.40432(10) 0.0512(6) Uani 1 1 d . . . . .
H43 H 0.9093 0.6407 0.3889 0.061 Uiso 1 1 calc R U . . .
C44 C 0.87840(19) 0.55543(16) 0.44340(11) 0.0614(7) Uani 1 1 d . . . . .
H44 H 0.9590 0.5449 0.4557 0.074 Uiso 1 1 calc R U . . .
C45 C 0.7915(2) 0.51361(17) 0.46453(10) 0.0660(7) Uani 1 1 d . . . . .
H45 H 0.8120 0.4735 0.4909 0.079 Uiso 1 1 calc R U . . .
C46 C 0.67329(19) 0.52983(14) 0.44745(9) 0.0490(5) Uani 1 1 d . . . . .
H46 H 0.6136 0.5004 0.4621 0.059 Uiso 1 1 calc R U . . .
C47 C 0.40876(15) 0.49950(10) 0.37088(7) 0.0299(4) Uani 1 1 d . . . . .
C48 C 0.31085(19) 0.47601(13) 0.39499(10) 0.0518(5) Uani 1 1 d . . . . .
H48 H 0.2712 0.5135 0.4149 0.062 Uiso 1 1 calc R U . . .
C49 C 0.2698(2) 0.39817(14) 0.39051(12) 0.0674(7) Uani 1 1 d . . . . .
H49 H 0.2028 0.3833 0.4074 0.081 Uiso 1 1 calc R U . . .
C50 C 0.3247(2) 0.34337(13) 0.36225(10) 0.0571(6) Uani 1 1 d . . . . .
H50 H 0.2963 0.2904 0.3593 0.068 Uiso 1 1 calc R U . . .
C51 C 0.4215(2) 0.36521(12) 0.33797(10) 0.0536(6) Uani 1 1 d . . . . .
H51 H 0.4601 0.3272 0.3180 0.064 Uiso 1 1 calc R U . . .
C52 C 0.46355(18) 0.44276(11) 0.34232(9) 0.0433(5) Uani 1 1 d . . . . .
H52 H 0.5309 0.4569 0.3254 0.052 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 C15 1.9440(15) . ?
Ge1 C21 1.9451(16) . ?
Ge1 C9 1.9618(16) . ?
Ge1 C1 1.9753(16) . ?
Ge2 C35 1.9421(16) . ?
Ge2 C41 1.9455(16) . ?
Ge2 C47 1.9619(16) . ?
Ge2 C27 1.9760(16) . ?
F1 C2 1.335(2) . ?
F2 C2 1.333(2) . ?
F3 C2 1.332(2) . ?
F4 C28 1.343(2) . ?
F5 C28 1.344(2) . ?
F6 C28 1.343(2) . ?
O1 C4 1.3464(19) . ?
O1 C5 1.451(2) . ?
O2 C4 1.2014(18) . ?
O3 C30 1.3480(19) . ?
O3 C31 1.452(2) . ?
O4 C30 1.2047(19) . ?
N1 C4 1.376(2) . ?
N1 C3 1.392(2) . ?
N1 C6 1.4796(19) . ?
N2 C30 1.377(2) . ?
N2 C29 1.3884(19) . ?
N2 C32 1.4851(19) . ?
C1 C3 1.340(2) . ?
C1 C2 1.485(2) . ?
C5 C6 1.533(2) . ?
C6 C7 1.516(2) . ?
C6 C8 1.518(2) . ?
C9 C14 1.383(2) . ?
C9 C10 1.390(2) . ?
C10 C11 1.392(3) . ?
C11 C12 1.377(3) . ?
C12 C13 1.370(3) . ?
C13 C14 1.390(3) . ?
C15 C20 1.392(2) . ?
C15 C16 1.398(2) . ?
C16 C17 1.381(2) . ?
C17 C18 1.381(3) . ?
C18 C19 1.379(3) . ?
C19 C20 1.389(2) . ?
C21 C22 1.390(3) . ?
C21 C26 1.393(3) . ?
C22 C23 1.387(3) . ?
C23 C24 1.373(4) . ?
C24 C25 1.375(4) . ?
C25 C26 1.397(3) . ?
C27 C29 1.338(2) . ?
C27 C28 1.493(2) . ?
C31 C32 1.530(2) . ?
C32 C34 1.525(2) . ?
C32 C33 1.525(2) . ?
C35 C40 1.391(3) . ?
C35 C36 1.394(2) . ?
C36 C37 1.385(3) . ?
C37 C38 1.382(3) . ?
C38 C39 1.379(3) . ?
C39 C40 1.384(3) . ?
C41 C42 1.386(2) . ?
C41 C46 1.392(3) . ?
C42 C43 1.387(3) . ?
C43 C44 1.381(3) . ?
C44 C45 1.372(4) . ?
C45 C46 1.392(3) . ?
C47 C52 1.384(3) . ?
C47 C48 1.387(3) . ?
C48 C49 1.394(3) . ?
C49 C50 1.358(4) . ?
C50 C51 1.371(3) . ?
C51 C52 1.393(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
C15 Ge1 C21 115.51(7) . . ?
C15 Ge1 C9 107.67(6) . . ?
C21 Ge1 C9 104.13(7) . . ?
C15 Ge1 C1 105.26(6) . . ?
C21 Ge1 C1 114.00(7) . . ?
C9 Ge1 C1 110.14(6) . . ?
C35 Ge2 C41 115.38(7) . . ?
C35 Ge2 C47 105.83(7) . . ?
C41 Ge2 C47 105.18(7) . . ?
C35 Ge2 C27 109.04(7) . . ?
C41 Ge2 C27 110.94(7) . . ?
C47 Ge2 C27 110.23(7) . . ?
C4 O1 C5 108.18(12) . . ?
C30 O3 C31 108.72(12) . . ?
C4 N1 C3 123.64(13) . . ?
C4 N1 C6 110.44(12) . . ?
C3 N1 C6 123.18(13) . . ?
C30 N2 C29 123.89(13) . . ?
C30 N2 C32 110.67(12) . . ?
C29 N2 C32 122.55(13) . . ?
C3 C1 C2 115.46(15) . . ?
C3 C1 Ge1 126.44(12) . . ?
C2 C1 Ge1 117.49(11) . . ?
F3 C2 F2 106.57(16) . . ?
F3 C2 F1 104.76(16) . . ?
F2 C2 F1 104.60(16) . . ?
F3 C2 C1 111.49(16) . . ?
F2 C2 C1 115.56(15) . . ?
F1 C2 C1 113.01(15) . . ?
C1 C3 N1 126.53(15) . . ?
O2 C4 O1 123.39(15) . . ?
O2 C4 N1 127.25(15) . . ?
O1 C4 N1 109.33(13) . . ?
O1 C5 C6 104.45(12) . . ?
N1 C6 C7 112.03(13) . . ?
N1 C6 C8 110.76(13) . . ?
C7 C6 C8 111.69(15) . . ?
N1 C6 C5 97.52(12) . . ?
C7 C6 C5 112.10(14) . . ?
C8 C6 C5 111.99(15) . . ?
C14 C9 C10 117.52(16) . . ?
C14 C9 Ge1 123.05(13) . . ?
C10 C9 Ge1 119.07(13) . . ?
C9 C10 C11 121.16(19) . . ?
C12 C11 C10 120.2(2) . . ?
C13 C12 C11 119.38(18) . . ?
C12 C13 C14 120.4(2) . . ?
C9 C14 C13 121.35(19) . . ?
C20 C15 C16 117.78(14) . . ?
C20 C15 Ge1 123.46(12) . . ?
C16 C15 Ge1 118.73(12) . . ?
C17 C16 C15 121.37(15) . . ?
C18 C17 C16 119.91(16) . . ?
C19 C18 C17 119.81(16) . . ?
C18 C19 C20 120.32(16) . . ?
C19 C20 C15 120.80(15) . . ?
C22 C21 C26 118.24(17) . . ?
C22 C21 Ge1 122.03(14) . . ?
C26 C21 Ge1 119.65(14) . . ?
C23 C22 C21 121.1(2) . . ?
C24 C23 C22 120.1(2) . . ?
C23 C24 C25 119.93(19) . . ?
C24 C25 C26 120.3(2) . . ?
C21 C26 C25 120.3(2) . . ?
C29 C27 C28 115.10(15) . . ?
C29 C27 Ge2 127.83(12) . . ?
C28 C27 Ge2 116.73(11) . . ?
F6 C28 F4 106.26(15) . . ?
F6 C28 F5 105.31(15) . . ?
F4 C28 F5 105.10(15) . . ?
F6 C28 C27 111.68(15) . . ?
F4 C28 C27 114.86(14) . . ?
F5 C28 C27 112.89(15) . . ?
C27 C29 N2 127.53(15) . . ?
O4 C30 O3 123.41(15) . . ?
O4 C30 N2 127.65(15) . . ?
O3 C30 N2 108.90(13) . . ?
O3 C31 C32 104.59(12) . . ?
N2 C32 C34 111.53(13) . . ?
N2 C32 C33 111.26(13) . . ?
C34 C32 C33 111.22(14) . . ?
N2 C32 C31 97.60(12) . . ?
C34 C32 C31 112.85(13) . . ?
C33 C32 C31 111.72(14) . . ?
C40 C35 C36 118.23(16) . . ?
C40 C35 Ge2 121.92(13) . . ?
C36 C35 Ge2 119.85(13) . . ?
C37 C36 C35 120.97(18) . . ?
C38 C37 C36 120.0(2) . . ?
C39 C38 C37 119.62(19) . . ?
C38 C39 C40 120.5(2) . . ?
C39 C40 C35 120.67(19) . . ?
C42 C41 C46 118.09(17) . . ?
C42 C41 Ge2 122.49(13) . . ?
C46 C41 Ge2 119.26(14) . . ?
C41 C42 C43 121.40(18) . . ?
C44 C43 C42 119.5(2) . . ?
C45 C44 C43 120.2(2) . . ?
C44 C45 C46 120.1(2) . . ?
C41 C46 C45 120.6(2) . . ?
C52 C47 C48 117.40(17) . . ?
C52 C47 Ge2 121.65(14) . . ?
C48 C47 Ge2 120.63(14) . . ?
C47 C48 C49 121.0(2) . . ?
C50 C49 C48 120.7(2) . . ?
C49 C50 C51 119.3(2) . . ?
C50 C51 C52 120.5(2) . . ?
C47 C52 C51 121.1(2) . . ?



################################################################################

data_Compound_40
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_formula_moiety          'C39 H33 Ge N O2'
_chemical_formula_sum             'C39 H33 Ge N O2'
_chemical_formula_weight          620.25

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'
 'O'  'O'   0.0106   0.0060
 '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/n'
_space_group_name_Hall            '-P 2yn'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, -y-1/2, z-1/2'
 
_cell_length_a                    11.0689(2)
_cell_length_b                    17.7248(3)
_cell_length_c                    16.4657(3)
_cell_angle_alpha                 90
_cell_angle_beta                  90.862(1)
_cell_angle_gamma                 90
_cell_volume                      3230.11(10)
_cell_formula_units_Z             4
_cell_measurement_temperature     200(2)
_cell_measurement_reflns_used     9907
_cell_measurement_theta_min       2.30
_cell_measurement_theta_max       29.87
 
_exptl_crystal_description        'fragment'
_exptl_crystal_colour             'colourless'
_exptl_crystal_size_max           0.55
_exptl_crystal_size_mid           0.38
_exptl_crystal_size_min           0.24
_exptl_crystal_density_method     'not measured'
_exptl_crystal_density_diffrn     1.275          
_exptl_crystal_F_000              1288
_exptl_absorpt_coefficient_mu     0.982
_exptl_absorpt_correction_type    numerical 
_exptl_absorpt_correction_T_min   0.704
_exptl_absorpt_correction_T_max   0.839
_exptl_absorpt_process_details     
; 
 SADABS : Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
; 
 
_diffrn_ambient_temperature       200(1)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   'curved graphite'
_diffrn_measurement_device_type   'Bruker APEX-II CCD'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_reflns_number             37208
_diffrn_reflns_av_unetI/netI      0.0255
_diffrn_reflns_av_R_equivalents   0.0218
_diffrn_reflns_limit_h_min        -15
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_k_min        -25
_diffrn_reflns_limit_k_max        20
_diffrn_reflns_limit_l_min        -23
_diffrn_reflns_limit_l_max        23
_diffrn_reflns_theta_min          1.688
_diffrn_reflns_theta_max          30.577
_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              9896
_reflns_number_gt                 7797
_reflns_threshold_expression      'I > 2σ(I)'
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;
 
_computing_data_collection        'Bruker APEX2'
_computing_cell_refinement        'Bruker SAINT'
_computing_data_reduction         'Bruker SAINT'
_computing_structure_solution     'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement   'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics     'SXGRAPH (Farrugia, 2012)'
_computing_publication_material   'WinGX (Farrugia, 2012)'

_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0476P)²+1.1848P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      dual
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_number_reflns          9896
_refine_ls_number_parameters      388
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0555
_refine_ls_R_factor_gt            0.0385
_refine_ls_wR_factor_ref          0.1016
_refine_ls_wR_factor_gt           0.0936
_refine_ls_goodness_of_fit_ref    1.075
_refine_ls_restrained_S_all       1.075
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
_refine_diff_density_max          1.104
_refine_diff_density_min         -0.387
_refine_diff_density_rms          0.056
 
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 0.20066(2) 0.19678(2) 0.62431(2) 0.02677(6) Uani 1 1 d . . . . .
O1 O 0.29711(13) 0.42195(7) 0.43841(7) 0.0397(3) Uani 1 1 d . . . . .
O2 O 0.35197(12) 0.52527(7) 0.50816(8) 0.0378(3) Uani 1 1 d . . . . .
N1 N 0.31660(12) 0.42074(7) 0.57755(8) 0.0263(3) Uani 1 1 d . . . . .
C1 C 0.20600(14) 0.30684(9) 0.61088(9) 0.0261(3) Uani 1 1 d . . . . .
C2 C 0.30835(14) 0.34039(9) 0.58594(9) 0.0260(3) Uani 1 1 d . . . . .
C3 C 0.31988(14) 0.45182(9) 0.50249(10) 0.0290(3) Uani 1 1 d . . . . .
C4 C 0.36771(19) 0.54530(11) 0.59221(12) 0.0421(4) Uani 1 1 d . . . . .
H4A H 0.3018 0.5791 0.6095 0.050 Uiso 1 1 calc R U . . .
H4B H 0.4457 0.5716 0.6008 0.050 Uiso 1 1 calc R U . . .
C5 C 0.36549(16) 0.47152(10) 0.64104(10) 0.0317(3) Uani 1 1 d . . . . .
C6 C 0.49191(19) 0.44809(13) 0.66848(13) 0.0481(5) Uani 1 1 d . . . . .
H6A H 0.5215 0.4829 0.7105 0.072 Uiso 1 1 calc R U . . .
H6B H 0.4895 0.3968 0.6906 0.072 Uiso 1 1 calc R U . . .
H6C H 0.5462 0.4495 0.6220 0.072 Uiso 1 1 calc R U . . .
C7 C 0.2812(2) 0.47717(14) 0.71289(13) 0.0551(6) Uani 1 1 d . . . . .
H7A H 0.3163 0.5112 0.7538 0.083 Uiso 1 1 calc R U . . .
H7B H 0.2028 0.4969 0.6944 0.083 Uiso 1 1 calc R U . . .
H7C H 0.2702 0.4270 0.7368 0.083 Uiso 1 1 calc R U . . .
C8 C 0.41327(15) 0.29931(9) 0.56131(10) 0.0299(3) Uani 1 1 d . . . . .
C9 C 0.49794(15) 0.26739(10) 0.53298(10) 0.0323(3) Uani 1 1 d . . . . .
C10 C 0.59683(16) 0.22880(10) 0.49630(10) 0.0342(4) Uani 1 1 d . . . . .
C11 C 0.5778(2) 0.16097(13) 0.45590(14) 0.0522(5) Uani 1 1 d . . . . .
H11 H 0.4994 0.1391 0.4536 0.063 Uiso 1 1 calc R U . . .
C12 C 0.6747(3) 0.12526(16) 0.41879(16) 0.0683(7) Uani 1 1 d . . . . .
H12 H 0.6615 0.0790 0.3908 0.082 Uiso 1 1 calc R U . . .
C13 C 0.7875(2) 0.15530(17) 0.42191(16) 0.0686(8) Uani 1 1 d . . . . .
H13 H 0.8527 0.1299 0.3970 0.082 Uiso 1 1 calc R U . . .
C14 C 0.8068(2) 0.22267(18) 0.46132(15) 0.0621(7) Uani 1 1 d . . . . .
H14 H 0.8856 0.2439 0.4631 0.074 Uiso 1 1 calc R U . . .
C15 C 0.71222(18) 0.26004(13) 0.49865(13) 0.0456(5) Uani 1 1 d . . . . .
H15 H 0.7262 0.3067 0.5256 0.055 Uiso 1 1 calc R U . . .
C16 C 0.09158(14) 0.34972(9) 0.61924(10) 0.0281(3) Uani 1 1 d . . . . .
C17 C 0.03881(15) 0.38321(11) 0.55067(11) 0.0361(4) Uani 1 1 d . . . . .
H17 H 0.0786 0.3807 0.5000 0.043 Uiso 1 1 calc R U . . .
C18 C -0.07107(17) 0.42001(12) 0.55593(15) 0.0480(5) Uani 1 1 d . . . . .
H18 H -0.1058 0.4430 0.5090 0.058 Uiso 1 1 calc R U . . .
C19 C -0.13049(17) 0.42351(12) 0.62880(16) 0.0499(5) Uani 1 1 d . . . . .
H19 H -0.2066 0.4480 0.6319 0.060 Uiso 1 1 calc R U . . .
C20 C -0.07907(17) 0.39136(11) 0.69689(14) 0.0440(5) Uani 1 1 d . . . . .
H20 H -0.1196 0.3943 0.7473 0.053 Uiso 1 1 calc R U . . .
C21 C 0.03162(16) 0.35461(10) 0.69284(11) 0.0349(4) Uani 1 1 d . . . . .
H21 H 0.0665 0.3328 0.7404 0.042 Uiso 1 1 calc R U . . .
C22 C 0.05464(15) 0.17525(9) 0.68446(10) 0.0297(3) Uani 1 1 d . . . . .
C23 C 0.05044(16) 0.18314(10) 0.76868(11) 0.0351(4) Uani 1 1 d . . . . .
H23 H 0.1232 0.1920 0.7985 0.042 Uiso 1 1 calc R U . . .
C24 C -0.05756(18) 0.17825(12) 0.80960(12) 0.0431(4) Uani 1 1 d . . . . .
H24 H -0.0587 0.1844 0.8669 0.052 Uiso 1 1 calc R U . . .
C25 C -0.16327(19) 0.16447(14) 0.76725(14) 0.0512(5) Uani 1 1 d . . . . .
H25 H -0.2375 0.1612 0.7953 0.061 Uiso 1 1 calc R U . . .
C26 C -0.16150(19) 0.15538(15) 0.68440(15) 0.0550(6) Uani 1 1 d . . . . .
H26 H -0.2345 0.1454 0.6553 0.066 Uiso 1 1 calc R U . . .
C27 C -0.05305(18) 0.16075(12) 0.64291(12) 0.0424(4) Uani 1 1 d . . . . .
H27 H -0.0527 0.1544 0.5856 0.051 Uiso 1 1 calc R U . . .
C28 C 0.34201(15) 0.15948(10) 0.68334(11) 0.0343(4) Uani 1 1 d . . . . .
C29 C 0.40770(19) 0.09894(12) 0.65435(15) 0.0490(5) Uani 1 1 d . . . . .
H29 H 0.3880 0.0779 0.6028 0.059 Uiso 1 1 calc R U . . .
C30 C 0.5030(2) 0.06866(15) 0.7007(2) 0.0696(8) Uani 1 1 d . . . . .
H30 H 0.5474 0.0271 0.6803 0.084 Uiso 1 1 calc R U . . .
C31 C 0.5329(2) 0.09820(16) 0.7749(2) 0.0711(9) Uani 1 1 d . . . . .
H31 H 0.5963 0.0765 0.8066 0.085 Uiso 1 1 calc R U . . .
C32 C 0.4707(2) 0.15927(18) 0.80307(17) 0.0677(7) Uani 1 1 d . . . . .
H32 H 0.4925 0.1808 0.8541 0.081 Uiso 1 1 calc R U . . .
C33 C 0.37565(19) 0.19031(13) 0.75763(14) 0.0488(5) Uani 1 1 d . . . . .
H33 H 0.3336 0.2329 0.7778 0.059 Uiso 1 1 calc R U . . .
C34 C 0.18657(16) 0.14996(10) 0.51791(11) 0.0354(4) Uani 1 1 d . . . . .
C35 C 0.1621(2) 0.07320(13) 0.51263(14) 0.0550(6) Uani 1 1 d . . . . .
H35 H 0.1506 0.0447 0.5608 0.066 Uiso 1 1 calc R U . . .
C36 C 0.1542(3) 0.03766(16) 0.43721(17) 0.0721(8) Uani 1 1 d . . . . .
H36 H 0.1381 -0.0149 0.4343 0.087 Uiso 1 1 calc R U . . .
C37 C 0.1695(3) 0.07808(18) 0.36768(15) 0.0693(8) Uani 1 1 d . . . . .
H37 H 0.1645 0.0535 0.3165 0.083 Uiso 1 1 calc R U . . .
C38 C 0.1921(2) 0.15394(16) 0.37136(13) 0.0593(6) Uani 1 1 d . . . . .
H38 H 0.2016 0.1819 0.3227 0.071 Uiso 1 1 calc R U . . .
C39 C 0.20118(19) 0.19035(12) 0.44624(11) 0.0422(4) Uani 1 1 d . . . . .
H39 H 0.2174 0.2429 0.4484 0.051 Uiso 1 1 calc R U . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Ge1 C34 1.9426(17) . ?
Ge1 C28 1.9453(17) . ?
Ge1 C22 1.9461(16) . ?
Ge1 C1 1.9642(16) . ?
O1 C3 1.204(2) . ?
O2 C3 1.352(2) . ?
O2 C4 1.437(2) . ?
N1 C3 1.354(2) . ?
N1 C2 1.434(2) . ?
N1 C5 1.476(2) . ?
C1 C2 1.349(2) . ?
C1 C16 1.485(2) . ?
C2 C8 1.434(2) . ?
C4 C5 1.535(3) . ?
C5 C7 1.521(3) . ?
C5 C6 1.522(3) . ?
C8 C9 1.196(2) . ?
C9 C10 1.432(2) . ?
C10 C11 1.389(3) . ?
C10 C15 1.392(3) . ?
C11 C12 1.394(3) . ?
C12 C13 1.358(4) . ?
C13 C14 1.374(4) . ?
C14 C15 1.390(3) . ?
C16 C21 1.393(2) . ?
C16 C17 1.396(2) . ?
C17 C18 1.384(3) . ?
C18 C19 1.378(3) . ?
C19 C20 1.374(3) . ?
C20 C21 1.390(3) . ?
C22 C27 1.389(2) . ?
C22 C23 1.395(2) . ?
C23 C24 1.384(3) . ?
C24 C25 1.375(3) . ?
C25 C26 1.374(3) . ?
C26 C27 1.393(3) . ?
C28 C29 1.385(3) . ?
C28 C33 1.386(3) . ?
C29 C30 1.400(3) . ?
C30 C31 1.365(4) . ?
C31 C32 1.368(4) . ?
C32 C33 1.395(3) . ?
C34 C35 1.390(3) . ?
C34 C39 1.392(3) . ?
C35 C36 1.394(3) . ?
C36 C37 1.363(4) . ?
C37 C38 1.369(4) . ?
C38 C39 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
C34 Ge1 C28 111.01(8) . . ?
C34 Ge1 C22 108.62(7) . . ?
C28 Ge1 C22 110.30(7) . . ?
C34 Ge1 C1 108.96(7) . . ?
C28 Ge1 C1 111.62(7) . . ?
C22 Ge1 C1 106.18(7) . . ?
C3 O2 C4 109.40(13) . . ?
C3 N1 C2 119.64(13) . . ?
C3 N1 C5 112.57(13) . . ?
C2 N1 C5 124.10(13) . . ?
C2 C1 C16 121.59(14) . . ?
C2 C1 Ge1 119.93(12) . . ?
C16 C1 Ge1 118.08(11) . . ?
C1 C2 N1 121.48(14) . . ?
C1 C2 C8 123.33(15) . . ?
N1 C2 C8 115.09(13) . . ?
O1 C3 O2 122.36(15) . . ?
O1 C3 N1 127.81(16) . . ?
O2 C3 N1 109.83(14) . . ?
O2 C4 C5 106.94(14) . . ?
N1 C5 C7 111.61(14) . . ?
N1 C5 C6 111.69(15) . . ?
C7 C5 C6 111.05(17) . . ?
N1 C5 C4 99.04(13) . . ?
C7 C5 C4 111.47(17) . . ?
C6 C5 C4 111.47(15) . . ?
C9 C8 C2 173.38(18) . . ?
C8 C9 C10 177.9(2) . . ?
C11 C10 C15 119.38(18) . . ?
C11 C10 C9 120.26(18) . . ?
C15 C10 C9 120.34(18) . . ?
C10 C11 C12 119.4(2) . . ?
C13 C12 C11 121.2(3) . . ?
C12 C13 C14 119.7(2) . . ?
C13 C14 C15 120.6(2) . . ?
C14 C15 C10 119.7(2) . . ?
C21 C16 C17 118.56(16) . . ?
C21 C16 C1 122.04(15) . . ?
C17 C16 C1 119.33(15) . . ?
C18 C17 C16 120.49(18) . . ?
C19 C18 C17 120.5(2) . . ?
C20 C19 C18 119.64(18) . . ?
C19 C20 C21 120.66(19) . . ?
C20 C21 C16 120.18(18) . . ?
C27 C22 C23 117.82(16) . . ?
C27 C22 Ge1 119.90(13) . . ?
C23 C22 Ge1 121.78(13) . . ?
C24 C23 C22 121.31(17) . . ?
C25 C24 C23 119.94(19) . . ?
C26 C25 C24 119.97(19) . . ?
C25 C26 C27 120.27(19) . . ?
C22 C27 C26 120.68(19) . . ?
C29 C28 C33 118.31(19) . . ?
C29 C28 Ge1 120.90(16) . . ?
C33 C28 Ge1 120.70(15) . . ?
C28 C29 C30 120.3(2) . . ?
C31 C30 C29 120.7(3) . . ?
C30 C31 C32 119.4(2) . . ?
C31 C32 C33 120.6(3) . . ?
C28 C33 C32 120.6(2) . . ?
C35 C34 C39 118.39(18) . . ?
C35 C34 Ge1 119.18(15) . . ?
C39 C34 Ge1 122.42(14) . . ?
C34 C35 C36 120.5(2) . . ?
C37 C36 C35 120.3(2) . . ?
C36 C37 C38 120.2(2) . . ?
C37 C38 C39 120.3(2) . . ?
C34 C39 C38 120.3(2) . . ?



################################################################################

data_Compound_44
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_formula_moiety          'C50 H48 Ge2 N2 O4 Zn, 2(C H2 Cl2)'
_chemical_formula_sum             'C52 H52 Cl4 Ge2 N2 O4 Zn'
_chemical_formula_weight          1121.30

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'
 'O'  'O'   0.0106   0.0060
 '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'
 'Zn'  'Zn'   0.2839   1.4301
 '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       orthorhombic
_space_group_IT_number            29
_space_group_name_H-M_alt         'P c a 21'
_space_group_name_Hall            'P 2c -2ac'
 
_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, z'
 '-x+1/2, y, z+1/2'
 
_cell_length_a                    21.4118(5)
_cell_length_b                    12.0493(2)
_cell_length_c                    39.1926(8)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      10111.6(4)
_cell_formula_units_Z             8
_cell_measurement_temperature     200(1)
_cell_measurement_reflns_used     9672
_cell_measurement_theta_min       2.17
_cell_measurement_theta_max       24.78
 
_exptl_crystal_description        'prism'
_exptl_crystal_colour             'colourless'
_exptl_crystal_size_max           0.32
_exptl_crystal_size_mid           0.07
_exptl_crystal_size_min           0.02
_exptl_crystal_density_method     'not measured'
_exptl_crystal_density_diffrn     1.473          
_exptl_crystal_F_000              4576
_exptl_absorpt_coefficient_mu     1.909
_exptl_absorpt_correction_type    numerical 
_exptl_absorpt_correction_T_min   0.699
_exptl_absorpt_correction_T_max   1.000
_exptl_absorpt_process_details     
; 
 SADABS : Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
; 
 
_diffrn_ambient_temperature       200(1)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   'curved graphite'
_diffrn_measurement_device_type   'Bruker APEX-II CCD'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_reflns_number             46305
_diffrn_reflns_av_unetI/netI      0.0597
_diffrn_reflns_av_R_equivalents   0.0439
_diffrn_reflns_limit_h_min        -26
_diffrn_reflns_limit_h_max        23
_diffrn_reflns_limit_k_min        -8
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -48
_diffrn_reflns_limit_l_max        43
_diffrn_reflns_theta_min          1.690
_diffrn_reflns_theta_max          26.391
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.998
_diffrn_measured_fraction_theta_full  0.999
_diffrn_reflns_Laue_measured_fraction_max    0.998
_diffrn_reflns_Laue_measured_fraction_full   0.999
_diffrn_reflns_point_group_measured_fraction_max   0.999
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              18058
_reflns_number_gt                 13862
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.969
_reflns_Friedel_fraction_max      0.999
_reflns_Friedel_fraction_full     1.000
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'Bruker APEX2'
_computing_cell_refinement        'Bruker SAINT'
_computing_data_reduction         'Bruker SAINT'
_computing_structure_solution     'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement   'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics     'SXGRAPH (Farrugia, 2012)'
_computing_publication_material   'WinGX (Farrugia, 2012)'

_refine_special_details
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0734P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      dual
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack    0.292(15)
_chemical_absolute_configuration  .
_refine_ls_number_reflns          18058
_refine_ls_number_parameters      1172
_refine_ls_number_restraints      13
_refine_ls_R_factor_all           0.0726
_refine_ls_R_factor_gt            0.0486
_refine_ls_wR_factor_ref          0.1260
_refine_ls_wR_factor_gt           0.1156
_refine_ls_goodness_of_fit_ref    1.023
_refine_ls_restrained_S_all       1.026
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
_refine_diff_density_max          0.683
_refine_diff_density_min         -0.858
_refine_diff_density_rms          0.087
 
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 0.28959(4) -0.10862(7) 0.14475(2) 0.0262(2) Uani 1 1 d . . . . .
Ge2 Ge 0.46355(4) 0.32200(8) 0.17267(2) 0.0299(2) Uani 1 1 d . . . . .
Ge3 Ge 0.52393(4) 0.60544(8) 0.40619(2) 0.0286(2) Uani 1 1 d . . . . .
Ge4 Ge 0.69592(4) 0.17146(7) 0.37998(2) 0.0268(2) Uani 1 1 d . . . . .
Zn1 Zn 0.42947(5) 0.06558(8) 0.11687(2) 0.0278(2) Uani 1 1 d . . . . .
Zn2 Zn 0.66309(5) 0.43184(8) 0.43453(3) 0.0286(2) Uani 1 1 d . . . . .
Cl1 Cl 0.0919(3) 0.4037(4) 0.04079(16) 0.137(2) Uani 1 1 d D . . . .
Cl2 Cl 0.2175(2) 0.4097(5) 0.01485(14) 0.1267(18) Uani 1 1 d D . . . .
Cl3 Cl 0.0518(2) 0.0954(4) 0.03372(13) 0.1093(15) Uani 1 1 d D . . . .
Cl4 Cl 0.1787(3) 0.1009(5) 0.01122(17) 0.152(2) Uani 1 1 d D . . . .
Cl5 Cl 0.2694(2) 0.1705(5) 0.26601(13) 0.1231(17) Uani 1 1 d D . . . .
Cl6 Cl 0.1470(2) 0.2105(4) 0.24011(14) 0.1114(15) Uani 1 1 d D . . . .
Cl7 Cl 0.5043(3) 0.2969(7) 0.29321(17) 0.173(3) Uani 1 1 d D . . . .
Cl8 Cl 0.3767(4) 0.2931(5) 0.31636(17) 0.160(2) Uani 1 1 d D . . . .
O1 O 0.5297(3) 0.0221(5) 0.1118(2) 0.0459(17) Uani 1 1 d . . . . .
O2 O 0.5879(3) -0.1249(6) 0.1235(2) 0.055(2) Uani 1 1 d . . . . .
O3 O 0.4042(4) 0.0539(5) 0.06237(16) 0.0460(17) Uani 1 1 d . . . . .
O4 O 0.3834(4) 0.1776(5) 0.02068(16) 0.052(2) Uani 1 1 d . . . . .
O5 O 0.7635(3) 0.4719(6) 0.4381(2) 0.0493(18) Uani 1 1 d . . . . .
O6 O 0.8223(3) 0.6191(6) 0.4255(2) 0.056(2) Uani 1 1 d . . . . .
O7 O 0.6381(4) 0.4448(5) 0.48895(16) 0.0449(17) Uani 1 1 d . . . . .
O8 O 0.6184(4) 0.3257(5) 0.53124(17) 0.051(2) Uani 1 1 d . . . . .
N1 N 0.4856(3) -0.1359(6) 0.13387(18) 0.0278(16) Uani 1 1 d . . . . .
N2 N 0.4111(3) 0.2421(5) 0.07187(17) 0.0291(16) Uani 1 1 d . . . . .
N3 N 0.7203(3) 0.6311(6) 0.4161(2) 0.0329(18) Uani 1 1 d . . . . .
N4 N 0.6457(3) 0.2586(6) 0.48042(17) 0.0290(16) Uani 1 1 d . . . . .
C1 C 0.4242(4) -0.0906(7) 0.1335(2) 0.0268(19) Uani 1 1 d . . . . .
C2 C 0.3746(4) -0.1542(7) 0.1413(2) 0.0262(18) Uani 1 1 d . . . . .
H2 H 0.3828 -0.2304 0.1456 0.031 Uiso 1 1 calc R U . . .
C3 C 0.5329(4) -0.0719(8) 0.1230(2) 0.033(2) Uani 1 1 d . . . . .
C4 C 0.5790(5) -0.2320(8) 0.1400(3) 0.055(3) Uani 1 1 d . . . . .
H4A H 0.5967 -0.2313 0.1633 0.066 Uiso 1 1 calc R U . . .
H4B H 0.5996 -0.2915 0.1267 0.066 Uiso 1 1 calc R U . . .
C5 C 0.5081(4) -0.2508(7) 0.1413(3) 0.037(2) Uani 1 1 d . . . . .
C6 C 0.4859(5) -0.3335(8) 0.1146(3) 0.051(3) Uani 1 1 d . . . . .
H6A H 0.5016 -0.4076 0.1203 0.076 Uiso 1 1 calc R U . . .
H6B H 0.4402 -0.3347 0.1142 0.076 Uiso 1 1 calc R U . . .
H6C H 0.5017 -0.3115 0.0921 0.076 Uiso 1 1 calc R U . . .
C7 C 0.4902(5) -0.2904(8) 0.1771(3) 0.046(3) Uani 1 1 d . . . . .
H7A H 0.5060 -0.3659 0.1807 0.069 Uiso 1 1 calc R U . . .
H7B H 0.5086 -0.2406 0.1942 0.069 Uiso 1 1 calc R U . . .
H7C H 0.4447 -0.2902 0.1795 0.069 Uiso 1 1 calc R U . . .
C8 C 0.2359(4) -0.1884(7) 0.1120(2) 0.030(2) Uani 1 1 d . . . . .
C9 C 0.1764(4) -0.1556(8) 0.1062(2) 0.036(2) Uani 1 1 d . . . . .
H9 H 0.1610 -0.0920 0.1178 0.043 Uiso 1 1 calc R U . . .
C10 C 0.1374(5) -0.2111(9) 0.0839(3) 0.045(2) Uani 1 1 d . . . . .
H10 H 0.0959 -0.1864 0.0802 0.054 Uiso 1 1 calc R U . . .
C11 C 0.1606(5) -0.3051(9) 0.0670(2) 0.049(3) Uani 1 1 d . . . . .
H11 H 0.1350 -0.3439 0.0513 0.059 Uiso 1 1 calc R U . . .
C12 C 0.2198(5) -0.3404(8) 0.0731(3) 0.046(3) Uani 1 1 d . . . . .
H12 H 0.2354 -0.4043 0.0618 0.055 Uiso 1 1 calc R U . . .
C13 C 0.2577(5) -0.2831(7) 0.0960(2) 0.037(2) Uani 1 1 d . . . . .
H13 H 0.2987 -0.3092 0.1006 0.045 Uiso 1 1 calc R U . . .
C14 C 0.2778(4) 0.0496(7) 0.1377(2) 0.028(2) Uani 1 1 d . . . . .
C15 C 0.2815(5) 0.1224(8) 0.1656(3) 0.042(2) Uani 1 1 d . . . . .
H15 H 0.2913 0.0949 0.1877 0.050 Uiso 1 1 calc R U . . .
C16 C 0.2705(5) 0.2363(8) 0.1606(3) 0.053(3) Uani 1 1 d . . . . .
H16 H 0.2740 0.2858 0.1794 0.064 Uiso 1 1 calc R U . . .
C17 C 0.2550(5) 0.2764(9) 0.1293(3) 0.053(3) Uani 1 1 d . . . . .
H17 H 0.2461 0.3530 0.1264 0.064 Uiso 1 1 calc R U . . .
C18 C 0.2524(5) 0.2067(9) 0.1023(3) 0.053(3) Uani 1 1 d . . . . .
H18 H 0.2430 0.2358 0.0804 0.064 Uiso 1 1 calc R U . . .
C19 C 0.2631(5) 0.0932(8) 0.1059(3) 0.042(2) Uani 1 1 d . . . . .
H19 H 0.2604 0.0457 0.0866 0.050 Uiso 1 1 calc R U . . .
C20 C 0.2638(4) -0.1450(7) 0.1911(2) 0.0287(19) Uani 1 1 d . . . . .
C21 C 0.2051(4) -0.1827(8) 0.2002(3) 0.040(2) Uani 1 1 d . . . . .
H21 H 0.1740 -0.1875 0.1830 0.048 Uiso 1 1 calc R U . . .
C22 C 0.1892(6) -0.2136(9) 0.2330(3) 0.060(3) Uani 1 1 d . . . . .
H22 H 0.1489 -0.2424 0.2380 0.072 Uiso 1 1 calc R U . . .
C23 C 0.2338(5) -0.2015(8) 0.2586(3) 0.044(3) Uani 1 1 d . . . . .
H23 H 0.2234 -0.2204 0.2814 0.053 Uiso 1 1 calc R U . . .
C24 C 0.2929(5) -0.1623(9) 0.2513(3) 0.048(3) Uani 1 1 d . . . . .
H24 H 0.3231 -0.1537 0.2689 0.058 Uiso 1 1 calc R U . . .
C25 C 0.3076(5) -0.1356(8) 0.2172(2) 0.039(2) Uani 1 1 d . . . . .
H25 H 0.3486 -0.1105 0.2119 0.047 Uiso 1 1 calc R U . . .
C26 C 0.4281(4) 0.2273(7) 0.1073(2) 0.0255(19) Uani 1 1 d . . . . .
C27 C 0.4457(5) 0.3169(7) 0.1247(2) 0.033(2) Uani 1 1 d . . . . .
H27 H 0.4498 0.3842 0.1123 0.040 Uiso 1 1 calc R U . . .
C28 C 0.4001(5) 0.1529(8) 0.0529(2) 0.040(2) Uani 1 1 d . . . . .
C29 C 0.3759(6) 0.2948(8) 0.0185(2) 0.046(3) Uani 1 1 d . . . . .
H29A H 0.3311 0.3145 0.0173 0.055 Uiso 1 1 calc R U . . .
H29B H 0.3971 0.3239 -0.0021 0.055 Uiso 1 1 calc R U . . .
C30 C 0.4057(5) 0.3436(7) 0.0509(2) 0.035(2) Uani 1 1 d . . . . .
C31 C 0.4696(5) 0.3920(9) 0.0430(3) 0.054(3) Uani 1 1 d . . . . .
H31A H 0.4647 0.4590 0.0291 0.081 Uiso 1 1 calc R U . . .
H31B H 0.4909 0.4108 0.0644 0.081 Uiso 1 1 calc R U . . .
H31C H 0.4945 0.3372 0.0304 0.081 Uiso 1 1 calc R U . . .
C32 C 0.3619(5) 0.4303(8) 0.0674(3) 0.048(3) Uani 1 1 d . . . . .
H32A H 0.3595 0.4961 0.0528 0.072 Uiso 1 1 calc R U . . .
H32B H 0.3201 0.3983 0.0701 0.072 Uiso 1 1 calc R U . . .
H32C H 0.3783 0.4513 0.0898 0.072 Uiso 1 1 calc R U . . .
C33 C 0.5443(4) 0.3988(7) 0.1784(2) 0.0302(19) Uani 1 1 d . . . . .
C34 C 0.5844(4) 0.4113(8) 0.1518(3) 0.046(3) Uani 1 1 d . . . . .
H34 H 0.5739 0.3793 0.1304 0.055 Uiso 1 1 calc R U . . .
C35 C 0.6392(5) 0.4683(10) 0.1547(3) 0.056(3) Uani 1 1 d . . . . .
H35 H 0.6659 0.4769 0.1355 0.067 Uiso 1 1 calc R U . . .
C36 C 0.6551(5) 0.5120(9) 0.1850(3) 0.057(3) Uani 1 1 d . . . . .
H36 H 0.6933 0.5514 0.1872 0.068 Uiso 1 1 calc R U . . .
C37 C 0.6165(5) 0.5004(8) 0.2128(3) 0.047(3) Uani 1 1 d . . . . .
H37 H 0.6278 0.5309 0.2343 0.057 Uiso 1 1 calc R U . . .
C38 C 0.5608(5) 0.4433(8) 0.2089(3) 0.043(2) Uani 1 1 d . . . . .
H38 H 0.5337 0.4351 0.2279 0.052 Uiso 1 1 calc R U . . .
C39 C 0.3995(4) 0.4154(8) 0.1940(3) 0.042(2) Uani 1 1 d . . . . .
C40 C 0.3624(4) 0.4819(9) 0.1730(4) 0.062(3) Uani 1 1 d . . . . .
H40 H 0.3688 0.4799 0.1490 0.075 Uiso 1 1 calc R U . . .
C41 C 0.3158(6) 0.5517(10) 0.1864(4) 0.066(4) Uani 1 1 d . . . . .
H41 H 0.2907 0.5966 0.1719 0.079 Uiso 1 1 calc R U . . .
C42 C 0.3083(6) 0.5522(11) 0.2197(5) 0.077(4) Uani 1 1 d . . . . .
H42 H 0.2767 0.5986 0.2290 0.092 Uiso 1 1 calc R U . . .
C43 C 0.3421(6) 0.4920(15) 0.2409(4) 0.089(5) Uani 1 1 d . . . . .
H43 H 0.3352 0.4968 0.2648 0.106 Uiso 1 1 calc R U . . .
C44 C 0.3900(6) 0.4184(12) 0.2276(3) 0.076(4) Uani 1 1 d . . . . .
H44 H 0.4140 0.3732 0.2425 0.092 Uiso 1 1 calc R U . . .
C45 C 0.4717(4) 0.1788(7) 0.1953(2) 0.034(2) Uani 1 1 d . . . . .
C46 C 0.4269(6) 0.1377(10) 0.2174(3) 0.060(3) Uani 1 1 d . . . . .
H46 H 0.3886 0.1762 0.2205 0.072 Uiso 1 1 calc R U . . .
C47 C 0.4385(9) 0.0384(14) 0.2351(4) 0.092(6) Uani 1 1 d . . . . .
H47 H 0.4086 0.0111 0.2509 0.111 Uiso 1 1 calc R U . . .
C48 C 0.4916(9) -0.0180(12) 0.2298(4) 0.079(5) Uani 1 1 d . . . . .
H48 H 0.4990 -0.0852 0.2418 0.095 Uiso 1 1 calc R U . . .
C49 C 0.5348(7) 0.0198(10) 0.2074(4) 0.070(4) Uani 1 1 d . . . . .
H49 H 0.5715 -0.0227 0.2035 0.084 Uiso 1 1 calc R U . . .
C50 C 0.5269(5) 0.1187(8) 0.1900(3) 0.049(3) Uani 1 1 d . . . . .
H50 H 0.5581 0.1453 0.1749 0.059 Uiso 1 1 calc R U . . .
C51 C 0.6581(4) 0.5858(7) 0.4168(2) 0.0261(19) Uani 1 1 d . . . . .
C52 C 0.6099(4) 0.6519(7) 0.4077(3) 0.033(2) Uani 1 1 d . . . . .
H52 H 0.6191 0.7265 0.4017 0.039 Uiso 1 1 calc R U . . .
C53 C 0.7679(4) 0.5649(9) 0.4276(3) 0.046(3) Uani 1 1 d . . . . .
C54 C 0.8129(5) 0.7230(10) 0.4110(4) 0.071(4) Uani 1 1 d . . . . .
H54A H 0.8327 0.7259 0.3882 0.086 Uiso 1 1 calc R U . . .
H54B H 0.8322 0.7809 0.4254 0.086 Uiso 1 1 calc R U . . .
C55 C 0.7417(4) 0.7448(7) 0.4076(3) 0.040(2) Uani 1 1 d . . . . .
C56 C 0.7270(6) 0.7801(10) 0.3711(3) 0.062(3) Uani 1 1 d . . . . .
H56A H 0.7417 0.7229 0.3552 0.094 Uiso 1 1 calc R U . . .
H56B H 0.6818 0.7895 0.3685 0.094 Uiso 1 1 calc R U . . .
H56C H 0.7481 0.8504 0.3661 0.094 Uiso 1 1 calc R U . . .
C57 C 0.7208(6) 0.8272(9) 0.4330(4) 0.064(4) Uani 1 1 d . . . . .
H57A H 0.7360 0.9010 0.4265 0.096 Uiso 1 1 calc R U . . .
H57B H 0.6751 0.8278 0.4340 0.096 Uiso 1 1 calc R U . . .
H57C H 0.7376 0.8076 0.4555 0.096 Uiso 1 1 calc R U . . .
C58 C 0.4726(4) 0.6880(7) 0.4384(2) 0.032(2) Uani 1 1 d . . . . .
C59 C 0.4959(5) 0.7806(8) 0.4563(2) 0.040(2) Uani 1 1 d . . . . .
H59 H 0.5379 0.8029 0.4527 0.047 Uiso 1 1 calc R U . . .
C60 C 0.4602(5) 0.8384(8) 0.4783(3) 0.053(3) Uani 1 1 d . . . . .
H60 H 0.4772 0.9010 0.4897 0.063 Uiso 1 1 calc R U . . .
C61 C 0.3985(6) 0.8070(10) 0.4844(3) 0.058(3) Uani 1 1 d . . . . .
H61 H 0.3733 0.8478 0.4999 0.070 Uiso 1 1 calc R U . . .
C62 C 0.3748(5) 0.7161(9) 0.4677(2) 0.042(2) Uani 1 1 d . . . . .
H62 H 0.3329 0.6938 0.4718 0.050 Uiso 1 1 calc R U . . .
C63 C 0.4109(4) 0.6573(8) 0.4452(2) 0.037(2) Uani 1 1 d . . . . .
H63 H 0.3937 0.5943 0.4341 0.044 Uiso 1 1 calc R U . . .
C64 C 0.4938(4) 0.6374(7) 0.3598(2) 0.031(2) Uani 1 1 d . . . . .
C65 C 0.5327(5) 0.6251(10) 0.3322(3) 0.053(3) Uani 1 1 d . . . . .
H65 H 0.5749 0.6036 0.3358 0.064 Uiso 1 1 calc R U . . .
C66 C 0.5116(6) 0.6435(12) 0.2992(3) 0.070(4) Uani 1 1 d . . . . .
H66 H 0.5395 0.6331 0.2806 0.084 Uiso 1 1 calc R U . . .
C67 C 0.4524(7) 0.6758(10) 0.2929(3) 0.070(4) Uani 1 1 d . . . . .
H67 H 0.4381 0.6871 0.2702 0.084 Uiso 1 1 calc R U . . .
C68 C 0.4134(5) 0.6920(10) 0.3201(3) 0.054(3) Uani 1 1 d . . . . .
H68 H 0.3720 0.7173 0.3162 0.065 Uiso 1 1 calc R U . . .
C69 C 0.4329(5) 0.6725(9) 0.3534(3) 0.046(2) Uani 1 1 d . . . . .
H69 H 0.4046 0.6829 0.3718 0.055 Uiso 1 1 calc R U . . .
C70 C 0.5121(4) 0.4467(7) 0.4154(2) 0.034(2) Uani 1 1 d . . . . .
C71 C 0.5180(5) 0.3722(9) 0.3901(3) 0.052(3) Uani 1 1 d . . . . .
H71 H 0.5297 0.3979 0.3681 0.062 Uiso 1 1 calc R U . . .
C72 C 0.5081(7) 0.2602(10) 0.3946(4) 0.070(4) Uani 1 1 d . . . . .
H72 H 0.5134 0.2100 0.3762 0.084 Uiso 1 1 calc R U . . .
C73 C 0.4905(5) 0.2228(9) 0.4257(4) 0.062(3) Uani 1 1 d . . . . .
H73 H 0.4814 0.1463 0.4290 0.074 Uiso 1 1 calc R U . . .
C74 C 0.4857(5) 0.2972(11) 0.4534(4) 0.066(4) Uani 1 1 d . . . . .
H74 H 0.4753 0.2711 0.4755 0.079 Uiso 1 1 calc R U . . .
C75 C 0.4966(5) 0.4105(8) 0.4475(3) 0.043(3) Uani 1 1 d . . . . .
H75 H 0.4932 0.4621 0.4658 0.052 Uiso 1 1 calc R U . . .
C76 C 0.6620(4) 0.2699(7) 0.4459(2) 0.0263(19) Uani 1 1 d . . . . .
C77 C 0.6786(4) 0.1796(7) 0.4274(2) 0.0274(19) Uani 1 1 d . . . . .
H77 H 0.6820 0.1120 0.4398 0.033 Uiso 1 1 calc R U . . .
C78 C 0.6347(5) 0.3499(8) 0.4992(2) 0.036(2) Uani 1 1 d . . . . .
C79 C 0.6110(6) 0.2068(8) 0.5337(3) 0.050(3) Uani 1 1 d . . . . .
H79A H 0.5661 0.1875 0.5352 0.059 Uiso 1 1 calc R U . . .
H79B H 0.6321 0.1789 0.5545 0.059 Uiso 1 1 calc R U . . .
C80 C 0.6402(4) 0.1536(7) 0.5018(2) 0.032(2) Uani 1 1 d . . . . .
C81 C 0.5965(5) 0.0707(7) 0.4867(2) 0.041(2) Uani 1 1 d . . . . .
H81A H 0.5563 0.1064 0.4820 0.061 Uiso 1 1 calc R U . . .
H81B H 0.6142 0.0418 0.4655 0.061 Uiso 1 1 calc R U . . .
H81C H 0.5903 0.0096 0.5029 0.061 Uiso 1 1 calc R U . . .
C82 C 0.7043(5) 0.1089(9) 0.5104(3) 0.049(3) Uani 1 1 d . . . . .
H82A H 0.7299 0.1685 0.5202 0.074 Uiso 1 1 calc R U . . .
H82B H 0.7003 0.0486 0.5270 0.074 Uiso 1 1 calc R U . . .
H82C H 0.7242 0.0808 0.4897 0.074 Uiso 1 1 calc R U . . .
C83 C 0.7764(4) 0.0984(7) 0.3744(2) 0.031(2) Uani 1 1 d . . . . .
C84 C 0.7950(5) 0.0543(8) 0.3431(3) 0.044(2) Uani 1 1 d . . . . .
H84 H 0.7684 0.0612 0.3238 0.053 Uiso 1 1 calc R U . . .
C85 C 0.8520(4) 0.0005(9) 0.3397(3) 0.051(3) Uani 1 1 d . . . . .
H85 H 0.8634 -0.0300 0.3182 0.061 Uiso 1 1 calc R U . . .
C86 C 0.8919(4) -0.0092(9) 0.3666(4) 0.056(3) Uani 1 1 d . . . . .
H86 H 0.9307 -0.0464 0.3639 0.067 Uiso 1 1 calc R U . . .
C87 C 0.8752(5) 0.0361(10) 0.3982(3) 0.060(3) Uani 1 1 d . . . . .
H87 H 0.9030 0.0303 0.4170 0.072 Uiso 1 1 calc R U . . .
C88 C 0.8179(4) 0.0896(8) 0.4022(3) 0.045(2) Uani 1 1 d . . . . .
H88 H 0.8069 0.1203 0.4237 0.053 Uiso 1 1 calc R U . . .
C89 C 0.6324(4) 0.0750(7) 0.3600(2) 0.034(2) Uani 1 1 d . . . . .
C90 C 0.5955(4) 0.0080(7) 0.3802(3) 0.035(2) Uani 1 1 d . . . . .
H90 H 0.6006 0.0119 0.4043 0.043 Uiso 1 1 calc R U . . .
C91 C 0.5519(5) -0.0641(9) 0.3673(3) 0.053(3) Uani 1 1 d . . . . .
H91 H 0.5280 -0.1093 0.3822 0.063 Uiso 1 1 calc R U . . .
C92 C 0.5428(5) -0.0707(10) 0.3322(4) 0.061(3) Uani 1 1 d . . . . .
H92 H 0.5126 -0.1202 0.3232 0.073 Uiso 1 1 calc R U . . .
C93 C 0.5772(6) -0.0064(12) 0.3110(3) 0.070(4) Uani 1 1 d . . . . .
H93 H 0.5710 -0.0109 0.2871 0.084 Uiso 1 1 calc R U . . .
C94 C 0.6231(5) 0.0685(10) 0.3245(3) 0.058(3) Uani 1 1 d . . . . .
H94 H 0.6471 0.1135 0.3095 0.070 Uiso 1 1 calc R U . . .
C95 C 0.7011(4) 0.3118(7) 0.3556(2) 0.033(2) Uani 1 1 d . . . . .
C96 C 0.7555(5) 0.3741(8) 0.3583(3) 0.048(3) Uani 1 1 d . . . . .
H96 H 0.7872 0.3516 0.3738 0.057 Uiso 1 1 calc R U . . .
C97 C 0.7640(7) 0.4677(10) 0.3390(4) 0.079(5) Uani 1 1 d . . . . .
H97 H 0.8014 0.5096 0.3412 0.095 Uiso 1 1 calc R U . . .
C98 C 0.7176(8) 0.5019(11) 0.3158(4) 0.083(5) Uani 1 1 d . . . . .
H98 H 0.7235 0.5652 0.3017 0.100 Uiso 1 1 calc R U . . .
C99 C 0.6639(6) 0.4410(10) 0.3142(3) 0.058(3) Uani 1 1 d . . . . .
H99 H 0.6313 0.4630 0.2992 0.069 Uiso 1 1 calc R U . . .
C100 C 0.6568(5) 0.3500(9) 0.3337(3) 0.047(3) Uani 1 1 d . . . . .
H100 H 0.6187 0.3101 0.3321 0.057 Uiso 1 1 calc R U . . .
C101 C 0.1406(6) 0.4194(14) 0.0063(4) 0.097(5) Uani 1 1 d D . . . .
H10A H 0.1298 0.3623 -0.0109 0.117 Uiso 1 1 calc R U . . .
H10B H 0.1324 0.4929 -0.0042 0.117 Uiso 1 1 calc R U . . .
C102 C 0.1292(6) 0.0941(14) 0.0442(4) 0.094(5) Uani 1 1 d D . . . .
H10C H 0.1377 0.1577 0.0596 0.113 Uiso 1 1 calc R U . . .
H10D H 0.1381 0.0254 0.0572 0.113 Uiso 1 1 calc R U . . .
C103 C 0.1969(7) 0.1148(13) 0.2550(5) 0.120(7) Uani 1 1 d D . . . .
H10E H 0.2030 0.0569 0.2374 0.144 Uiso 1 1 calc R U . . .
H10F H 0.1784 0.0788 0.2753 0.144 Uiso 1 1 calc R U . . .
C104 C 0.4373(7) 0.3716(15) 0.3127(4) 0.120(7) Uani 1 1 d D . . . .
H10G H 0.4496 0.3991 0.3355 0.144 Uiso 1 1 calc R U . . .
H10H H 0.4267 0.4367 0.2984 0.144 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 C2 1.905(8) . ?
Ge1 C14 1.943(8) . ?
Ge1 C20 1.950(9) . ?
Ge1 C8 1.973(8) . ?
Ge2 C27 1.920(9) . ?
Ge2 C45 1.948(9) . ?
Ge2 C39 1.961(9) . ?
Ge2 C33 1.974(9) . ?
Ge3 C52 1.925(8) . ?
Ge3 C58 1.948(9) . ?
Ge3 C70 1.963(9) . ?
Ge3 C64 1.969(9) . ?
Ge4 C77 1.899(8) . ?
Ge4 C95 1.946(9) . ?
Ge4 C83 1.948(8) . ?
Ge4 C89 1.953(10) . ?
Zn1 C26 1.985(8) . ?
Zn1 C1 1.995(8) . ?
Zn1 O3 2.208(6) . ?
Zn1 O1 2.218(6) . ?
Zn2 C51 1.983(8) . ?
Zn2 C76 2.002(8) . ?
Zn2 O7 2.205(6) . ?
Zn2 O5 2.209(7) . ?
Cl1 C101 1.719(14) . ?
Cl2 C101 1.686(13) . ?
Cl3 C102 1.708(12) . ?
Cl4 C102 1.674(14) . ?
Cl5 C103 1.745(15) . ?
Cl6 C103 1.676(15) . ?
Cl7 C104 1.857(16) . ?
Cl8 C104 1.614(16) . ?
O1 C3 1.216(10) . ?
O2 C3 1.339(10) . ?
O2 C4 1.456(12) . ?
O3 C28 1.252(11) . ?
O4 C28 1.347(11) . ?
O4 C29 1.424(11) . ?
O5 C53 1.197(11) . ?
O6 C53 1.337(11) . ?
O6 C54 1.390(13) . ?
O7 C78 1.214(11) . ?
O8 C78 1.335(11) . ?
O8 C79 1.446(12) . ?
N1 C3 1.342(11) . ?
N1 C1 1.422(10) . ?
N1 C5 1.495(10) . ?
N2 C28 1.327(12) . ?
N2 C26 1.445(10) . ?
N2 C30 1.479(10) . ?
N3 C53 1.372(12) . ?
N3 C51 1.439(10) . ?
N3 C55 1.483(11) . ?
N4 C78 1.344(11) . ?
N4 C76 1.405(10) . ?
N4 C80 1.522(11) . ?
C1 C2 1.346(11) . ?
C4 C5 1.534(13) . ?
C5 C6 1.519(13) . ?
C5 C7 1.534(14) . ?
C8 C9 1.353(12) . ?
C8 C13 1.383(12) . ?
C9 C10 1.380(13) . ?
C10 C11 1.403(15) . ?
C11 C12 1.358(14) . ?
C12 C13 1.393(13) . ?
C14 C19 1.390(12) . ?
C14 C15 1.404(13) . ?
C15 C16 1.405(14) . ?
C16 C17 1.361(16) . ?
C17 C18 1.351(16) . ?
C18 C19 1.394(14) . ?
C20 C21 1.383(12) . ?
C20 C25 1.393(12) . ?
C21 C22 1.382(15) . ?
C22 C23 1.392(16) . ?
C23 C24 1.381(15) . ?
C24 C25 1.409(14) . ?
C26 C27 1.333(12) . ?
C29 C30 1.537(13) . ?
C30 C31 1.519(13) . ?
C30 C32 1.545(14) . ?
C33 C38 1.358(13) . ?
C33 C34 1.359(13) . ?
C34 C35 1.365(13) . ?
C35 C36 1.342(16) . ?
C36 C37 1.375(16) . ?
C37 C38 1.385(13) . ?
C39 C44 1.331(16) . ?
C39 C40 1.398(15) . ?
C40 C41 1.406(16) . ?
C41 C42 1.32(2) . ?
C42 C43 1.32(2) . ?
C43 C44 1.453(18) . ?
C45 C46 1.383(14) . ?
C45 C50 1.401(13) . ?
C46 C47 1.406(19) . ?
C47 C48 1.34(2) . ?
C48 C49 1.35(2) . ?
C49 C50 1.383(15) . ?
C51 C52 1.351(11) . ?
C54 C55 1.552(14) . ?
C55 C57 1.477(16) . ?
C55 C56 1.525(16) . ?
C58 C63 1.398(12) . ?
C58 C59 1.408(13) . ?
C59 C60 1.346(14) . ?
C60 C61 1.395(15) . ?
C61 C62 1.373(15) . ?
C62 C63 1.370(13) . ?
C64 C65 1.372(14) . ?
C64 C69 1.394(13) . ?
C65 C66 1.389(16) . ?
C66 C67 1.348(18) . ?
C67 C68 1.369(18) . ?
C68 C69 1.389(14) . ?
C70 C71 1.342(14) . ?
C70 C75 1.374(13) . ?
C71 C72 1.377(16) . ?
C72 C73 1.352(18) . ?
C73 C74 1.410(18) . ?
C74 C75 1.404(15) . ?
C76 C77 1.353(12) . ?
C79 C80 1.538(13) . ?
C80 C81 1.491(13) . ?
C80 C82 1.512(13) . ?
C83 C84 1.396(12) . ?
C83 C88 1.409(13) . ?
C84 C85 1.388(13) . ?
C85 C86 1.360(16) . ?
C86 C87 1.399(17) . ?
C87 C88 1.395(14) . ?
C89 C90 1.381(13) . ?
C89 C94 1.406(14) . ?
C90 C91 1.373(13) . ?
C91 C92 1.389(17) . ?
C92 C93 1.355(18) . ?
C93 C94 1.435(15) . ?
C95 C100 1.357(13) . ?
C95 C96 1.390(13) . ?
C96 C97 1.371(15) . ?
C97 C98 1.41(2) . ?
C98 C99 1.365(19) . ?
C99 C100 1.347(15) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
C2 Ge1 C14 113.4(3) . . ?
C2 Ge1 C20 105.8(4) . . ?
C14 Ge1 C20 108.4(4) . . ?
C2 Ge1 C8 111.7(4) . . ?
C14 Ge1 C8 108.1(4) . . ?
C20 Ge1 C8 109.4(3) . . ?
C27 Ge2 C45 115.8(4) . . ?
C27 Ge2 C39 107.3(4) . . ?
C45 Ge2 C39 112.1(4) . . ?
C27 Ge2 C33 107.5(4) . . ?
C45 Ge2 C33 106.5(4) . . ?
C39 Ge2 C33 107.2(4) . . ?
C52 Ge3 C58 111.8(4) . . ?
C52 Ge3 C70 113.6(4) . . ?
C58 Ge3 C70 107.8(4) . . ?
C52 Ge3 C64 106.6(4) . . ?
C58 Ge3 C64 108.3(4) . . ?
C70 Ge3 C64 108.6(4) . . ?
C77 Ge4 C95 116.6(4) . . ?
C77 Ge4 C83 107.9(4) . . ?
C95 Ge4 C83 106.7(3) . . ?
C77 Ge4 C89 106.7(4) . . ?
C95 Ge4 C89 111.0(4) . . ?
C83 Ge4 C89 107.6(4) . . ?
C26 Zn1 C1 170.9(3) . . ?
C26 Zn1 O3 82.8(3) . . ?
C1 Zn1 O3 104.0(3) . . ?
C26 Zn1 O1 103.3(3) . . ?
C1 Zn1 O1 82.0(3) . . ?
O3 Zn1 O1 97.8(3) . . ?
C51 Zn2 C76 171.4(3) . . ?
C51 Zn2 O7 105.1(3) . . ?
C76 Zn2 O7 81.5(3) . . ?
C51 Zn2 O5 82.6(3) . . ?
C76 Zn2 O5 102.2(3) . . ?
O7 Zn2 O5 99.2(3) . . ?
C3 O1 Zn1 104.1(6) . . ?
C3 O2 C4 108.3(7) . . ?
C28 O3 Zn1 104.0(6) . . ?
C28 O4 C29 107.8(7) . . ?
C53 O5 Zn2 105.1(6) . . ?
C53 O6 C54 109.8(8) . . ?
C78 O7 Zn2 105.5(6) . . ?
C78 O8 C79 108.0(7) . . ?
C3 N1 C1 118.3(7) . . ?
C3 N1 C5 110.4(7) . . ?
C1 N1 C5 130.9(7) . . ?
C28 N2 C26 118.8(7) . . ?
C28 N2 C30 110.2(7) . . ?
C26 N2 C30 131.0(7) . . ?
C53 N3 C51 117.5(7) . . ?
C53 N3 C55 112.3(7) . . ?
C51 N3 C55 129.9(7) . . ?
C78 N4 C76 119.5(7) . . ?
C78 N4 C80 111.4(7) . . ?
C76 N4 C80 129.1(7) . . ?
C2 C1 N1 120.6(8) . . ?
C2 C1 Zn1 131.0(6) . . ?
N1 C1 Zn1 108.2(6) . . ?
C1 C2 Ge1 127.3(6) . . ?
O1 C3 O2 119.9(8) . . ?
O1 C3 N1 127.3(8) . . ?
O2 C3 N1 112.7(8) . . ?
O2 C4 C5 106.0(7) . . ?
N1 C5 C6 111.9(8) . . ?
N1 C5 C4 100.2(7) . . ?
C6 C5 C4 112.5(8) . . ?
N1 C5 C7 112.7(8) . . ?
C6 C5 C7 110.3(8) . . ?
C4 C5 C7 108.8(8) . . ?
C9 C8 C13 118.9(8) . . ?
C9 C8 Ge1 121.0(7) . . ?
C13 C8 Ge1 120.0(7) . . ?
C8 C9 C10 122.3(9) . . ?
C9 C10 C11 118.4(10) . . ?
C12 C11 C10 120.0(9) . . ?
C11 C12 C13 120.1(9) . . ?
C8 C13 C12 120.2(9) . . ?
C19 C14 C15 118.4(8) . . ?
C19 C14 Ge1 121.9(7) . . ?
C15 C14 Ge1 119.7(7) . . ?
C14 C15 C16 119.5(10) . . ?
C17 C16 C15 120.8(10) . . ?
C18 C17 C16 119.7(9) . . ?
C17 C18 C19 121.7(10) . . ?
C14 C19 C18 119.8(10) . . ?
C21 C20 C25 116.7(9) . . ?
C21 C20 Ge1 124.9(7) . . ?
C25 C20 Ge1 118.4(7) . . ?
C22 C21 C20 123.5(10) . . ?
C21 C22 C23 118.2(10) . . ?
C24 C23 C22 121.1(10) . . ?
C23 C24 C25 118.6(10) . . ?
C20 C25 C24 121.8(9) . . ?
C27 C26 N2 117.6(8) . . ?
C27 C26 Zn1 133.9(7) . . ?
N2 C26 Zn1 107.9(5) . . ?
C26 C27 Ge2 125.8(7) . . ?
O3 C28 N2 126.4(9) . . ?
O3 C28 O4 120.4(8) . . ?
N2 C28 O4 113.2(8) . . ?
O4 C29 C30 106.4(7) . . ?
N2 C30 C31 111.1(8) . . ?
N2 C30 C29 100.1(7) . . ?
C31 C30 C29 110.6(8) . . ?
N2 C30 C32 111.9(7) . . ?
C31 C30 C32 111.9(8) . . ?
C29 C30 C32 110.7(8) . . ?
C38 C33 C34 117.9(9) . . ?
C38 C33 Ge2 120.9(7) . . ?
C34 C33 Ge2 121.2(7) . . ?
C33 C34 C35 122.3(10) . . ?
C36 C35 C34 119.4(10) . . ?
C35 C36 C37 120.5(10) . . ?
C36 C37 C38 118.8(10) . . ?
C33 C38 C37 121.1(10) . . ?
C44 C39 C40 118.6(11) . . ?
C44 C39 Ge2 123.0(9) . . ?
C40 C39 Ge2 118.4(8) . . ?
C39 C40 C41 121.9(13) . . ?
C42 C41 C40 117.3(14) . . ?
C41 C42 C43 123.8(13) . . ?
C42 C43 C44 119.6(14) . . ?
C39 C44 C43 118.8(13) . . ?
C46 C45 C50 119.5(10) . . ?
C46 C45 Ge2 122.7(9) . . ?
C50 C45 Ge2 117.8(7) . . ?
C45 C46 C47 119.3(14) . . ?
C48 C47 C46 120.4(15) . . ?
C47 C48 C49 120.6(14) . . ?
C48 C49 C50 121.6(14) . . ?
C49 C50 C45 118.5(11) . . ?
C52 C51 N3 118.5(7) . . ?
C52 C51 Zn2 133.3(6) . . ?
N3 C51 Zn2 108.1(6) . . ?
C51 C52 Ge3 124.5(6) . . ?
O5 C53 O6 123.1(9) . . ?
O5 C53 N3 126.8(9) . . ?
O6 C53 N3 110.1(8) . . ?
O6 C54 C55 109.3(8) . . ?
C57 C55 N3 112.1(8) . . ?
C57 C55 C56 112.5(9) . . ?
N3 C55 C56 113.8(9) . . ?
C57 C55 C54 110.7(10) . . ?
N3 C55 C54 97.4(7) . . ?
C56 C55 C54 109.2(9) . . ?
C63 C58 C59 116.7(9) . . ?
C63 C58 Ge3 121.5(7) . . ?
C59 C58 Ge3 121.8(7) . . ?
C60 C59 C58 121.8(9) . . ?
C59 C60 C61 120.5(10) . . ?
C62 C61 C60 119.0(10) . . ?
C63 C62 C61 120.7(10) . . ?
C62 C63 C58 121.3(9) . . ?
C65 C64 C69 117.4(9) . . ?
C65 C64 Ge3 120.5(7) . . ?
C69 C64 Ge3 122.0(7) . . ?
C64 C65 C66 121.3(11) . . ?
C67 C66 C65 121.4(11) . . ?
C66 C67 C68 118.2(11) . . ?
C67 C68 C69 121.7(11) . . ?
C68 C69 C64 119.9(10) . . ?
C71 C70 C75 119.2(9) . . ?
C71 C70 Ge3 120.3(8) . . ?
C75 C70 Ge3 120.6(7) . . ?
C70 C71 C72 123.1(12) . . ?
C73 C72 C71 119.0(12) . . ?
C72 C73 C74 120.0(11) . . ?
C75 C74 C73 118.7(11) . . ?
C70 C75 C74 119.9(11) . . ?
C77 C76 N4 120.1(7) . . ?
C77 C76 Zn2 131.5(6) . . ?
N4 C76 Zn2 108.1(6) . . ?
C76 C77 Ge4 128.0(6) . . ?
O7 C78 O8 122.2(8) . . ?
O7 C78 N4 125.4(8) . . ?
O8 C78 N4 112.5(8) . . ?
O8 C79 C80 108.3(7) . . ?
C81 C80 C82 114.8(8) . . ?
C81 C80 N4 112.7(7) . . ?
C82 C80 N4 110.4(8) . . ?
C81 C80 C79 110.3(8) . . ?
C82 C80 C79 109.6(8) . . ?
N4 C80 C79 97.7(7) . . ?
C84 C83 C88 118.1(9) . . ?
C84 C83 Ge4 121.6(7) . . ?
C88 C83 Ge4 120.4(7) . . ?
C85 C84 C83 120.8(10) . . ?
C86 C85 C84 121.2(10) . . ?
C85 C86 C87 119.5(10) . . ?
C88 C87 C86 120.3(10) . . ?
C87 C88 C83 120.2(10) . . ?
C90 C89 C94 117.0(9) . . ?
C90 C89 Ge4 121.0(7) . . ?
C94 C89 Ge4 121.9(7) . . ?
C91 C90 C89 123.2(10) . . ?
C90 C91 C92 119.8(11) . . ?
C93 C92 C91 119.9(11) . . ?
C92 C93 C94 120.4(12) . . ?
C89 C94 C93 119.8(11) . . ?
C100 C95 C96 116.8(9) . . ?
C100 C95 Ge4 124.4(8) . . ?
C96 C95 Ge4 118.6(7) . . ?
C97 C96 C95 120.9(12) . . ?
C96 C97 C98 120.2(13) . . ?
C99 C98 C97 117.8(11) . . ?
C100 C99 C98 120.4(12) . . ?
C99 C100 C95 123.9(11) . . ?
Cl2 C101 Cl1 115.3(9) . . ?
Cl4 C102 Cl3 115.3(9) . . ?
Cl6 C103 Cl5 112.8(9) . . ?
Cl8 C104 Cl7 112.0(10) . . ?



################################################################################

data_Compound_45
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_formula_moiety          'C52 H52 Ge2 N2 O4 Zn, 2(C H2 Cl2)'
_chemical_formula_sum             'C54 H56 Cl4 Ge2 N2 O4 Zn'
_chemical_formula_weight          1149.35

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0181   0.0091
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0311   0.0180
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0492   0.0322
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.3639   0.7018
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn'  'Zn'  -1.5491   0.6778
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ge'  'Ge'  -1.0885   0.8855
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            19
_space_group_name_H-M_alt         'P 21 21 21'
_space_group_name_Hall            'P 2ac 2ab'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 '-x, y+1/2, -z+1/2'
 'x+1/2, -y+1/2, -z'
 
_cell_length_a                    13.4291(6)
_cell_length_b                    17.2102(8)
_cell_length_c                    23.7226(12)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      5482.7(4)
_cell_formula_units_Z             4
_cell_measurement_temperature     200(1)
_cell_measurement_reflns_used     6671
_cell_measurement_theta_min       3.73
_cell_measurement_theta_max       66.47
 
_exptl_crystal_description        'plate fragment'
_exptl_crystal_colour             'colourless'
_exptl_crystal_size_max           0.39
_exptl_crystal_size_mid           0.18
_exptl_crystal_size_min           0.02
_exptl_crystal_density_method     'not measured'
_exptl_crystal_density_diffrn     1.392          
_exptl_crystal_F_000              2352
_exptl_absorpt_coefficient_mu     3.946
_exptl_absorpt_correction_type    numerical 
_exptl_absorpt_correction_T_min   0.535
_exptl_absorpt_correction_T_max   1.000
_exptl_absorpt_process_details     
; 
 SADABS : Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
; 
 
_diffrn_ambient_temperature       200(1)
_diffrn_radiation_wavelength      1.54178
_diffrn_radiation_type            CuK\a
_diffrn_radiation_source          'micro-source'
_diffrn_measurement_device_type   'Bruker APEX-II CCD'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_reflns_number             25916
_diffrn_reflns_av_unetI/netI      0.0995
_diffrn_reflns_av_R_equivalents   0.0935
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_k_min        -20
_diffrn_reflns_limit_k_max        20
_diffrn_reflns_limit_l_min        -28
_diffrn_reflns_limit_l_max        28
_diffrn_reflns_theta_min          3.172
_diffrn_reflns_theta_max          66.925
_diffrn_reflns_theta_full         66.500
_diffrn_measured_fraction_theta_max   0.995
_diffrn_measured_fraction_theta_full  0.998
_diffrn_reflns_Laue_measured_fraction_max    0.995
_diffrn_reflns_Laue_measured_fraction_full   0.998
_diffrn_reflns_point_group_measured_fraction_max   0.976
_diffrn_reflns_point_group_measured_fraction_full  0.981
_reflns_number_total              9520
_reflns_number_gt                 7772
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.773
_reflns_Friedel_fraction_max      0.953
_reflns_Friedel_fraction_full     0.960
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'Bruker APEX2'
_computing_cell_refinement        'Bruker SAINT'
_computing_data_reduction         'Bruker SAINT'
_computing_structure_solution     'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement   'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics     'SXGRAPH (Farrugia, 2012)'
_computing_publication_material   'WinGX (Farrugia, 2012)'

_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0848P)²+1.3550P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      dual
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_abs_structure_details
;
 Flack x determined using 2709 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack    0.02(2)
_chemical_absolute_configuration  ad
_refine_ls_number_reflns          9520
_refine_ls_number_parameters      622
_refine_ls_number_restraints      10
_refine_ls_R_factor_all           0.0776
_refine_ls_R_factor_gt            0.0628
_refine_ls_wR_factor_ref          0.1732
_refine_ls_wR_factor_gt           0.1609
_refine_ls_goodness_of_fit_ref    1.040
_refine_ls_restrained_S_all       1.045
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
_refine_diff_density_max          0.996
_refine_diff_density_min         -0.793
_refine_diff_density_rms          0.094
 
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 0.17284(6) 0.58112(5) 0.47859(4) 0.0429(2) Uani 1 1 d . . . . .
Ge2 Ge 0.58471(6) 0.42412(5) 0.47132(4) 0.0437(2) Uani 1 1 d . . . . .
Zn1 Zn 0.37864(8) 0.49931(5) 0.56996(5) 0.0483(3) Uani 1 1 d . . . . .
Cl1 Cl 0.3924(5) 0.9914(3) 0.6981(3) 0.179(3) Uani 1 1 d D . . . .
Cl2 Cl 0.2909(4) 1.0031(4) 0.8045(2) 0.190(3) Uani 1 1 d D . . . .
Cl3A Cl 0.1362(5) 0.5215(5) 0.7773(3) 0.196(3) Uani 0.4 1 d D . P A 1
Cl4A Cl -0.0163(7) 0.4281(7) 0.7299(6) 0.123(4) Uani 0.4 1 d D . P A 1
Cl3B Cl 0.1362(5) 0.5215(5) 0.7773(3) 0.196(3) Uani 0.4 1 d D . P B 2
Cl4B Cl 0.0218(11) 0.4635(9) 0.6871(6) 0.153(5) Uani 0.4 1 d D . P B 2
Cl3C Cl 0.1362(5) 0.5215(5) 0.7773(3) 0.196(3) Uani 0.2 1 d D . P C 3
Cl4C Cl 0.041(2) 0.3931(13) 0.7811(10) 0.155(11) Uani 0.2 1 d D . P C 3
O1 O 0.4704(6) 0.5557(4) 0.6384(3) 0.0698(19) Uani 1 1 d . . . . .
O2 O 0.4812(6) 0.6776(4) 0.6721(3) 0.073(2) Uani 1 1 d . . . . .
O3 O 0.2868(5) 0.4352(4) 0.6342(3) 0.0594(15) Uani 1 1 d . . . . .
O4 O 0.2773(5) 0.3110(4) 0.6608(3) 0.0593(16) Uani 1 1 d . . . . .
N1 N 0.3722(5) 0.6535(4) 0.6041(3) 0.0480(16) Uani 1 1 d . . . . .
N2 N 0.3861(5) 0.3417(4) 0.5936(3) 0.0429(15) Uani 1 1 d . . . . .
C1 C 0.3236(6) 0.6062(4) 0.5633(3) 0.0430(17) Uani 1 1 d . . . . .
C2 C 0.2552(6) 0.6377(4) 0.5296(3) 0.0438(17) Uani 1 1 d . . . . .
H2 H 0.2469 0.6925 0.5311 0.053 Uiso 1 1 calc R U . . .
C3 C 0.4416(8) 0.6223(5) 0.6374(4) 0.057(2) Uani 1 1 d . . . . .
C4 C 0.4404(9) 0.7524(6) 0.6565(5) 0.077(3) Uani 1 1 d . . . . .
H4A H 0.4896 0.7829 0.6347 0.093 Uiso 1 1 calc R U . . .
H4B H 0.4213 0.7824 0.6904 0.093 Uiso 1 1 calc R U . . .
C5 C 0.3481(7) 0.7342(5) 0.6201(4) 0.058(2) Uani 1 1 d . . . . .
H5 H 0.3487 0.7678 0.5857 0.069 Uiso 1 1 calc R U . . .
C6 C 0.2484(9) 0.7420(7) 0.6496(5) 0.081(3) Uani 1 1 d . . . . .
H6 H 0.1959 0.7230 0.6230 0.097 Uiso 1 1 calc R U . . .
C7 C 0.2429(11) 0.6930(10) 0.7018(6) 0.119(6) Uani 1 1 d . . . . .
H7A H 0.1775 0.6996 0.7196 0.178 Uiso 1 1 calc R U . . .
H7B H 0.2524 0.6382 0.6918 0.178 Uiso 1 1 calc R U . . .
H7C H 0.2951 0.7091 0.7282 0.178 Uiso 1 1 calc R U . . .
C8 C 0.2285(13) 0.8283(9) 0.6607(7) 0.139(7) Uani 1 1 d . . . . .
H8A H 0.2331 0.8572 0.6252 0.208 Uiso 1 1 calc R U . . .
H8B H 0.1617 0.8347 0.6766 0.208 Uiso 1 1 calc R U . . .
H8C H 0.2780 0.8484 0.6873 0.208 Uiso 1 1 calc R U . . .
C9 C 0.2056(5) 0.4708(4) 0.4728(4) 0.0439(17) Uani 1 1 d . . . . .
C10 C 0.1679(6) 0.4181(5) 0.5124(4) 0.0536(19) Uani 1 1 d . . . . .
H10 H 0.1278 0.4367 0.5425 0.064 Uiso 1 1 calc R U . . .
C11 C 0.1879(7) 0.3401(5) 0.5085(4) 0.063(2) Uani 1 1 d . . . . .
H11 H 0.1620 0.3054 0.5360 0.075 Uiso 1 1 calc R U . . .
C12 C 0.2447(8) 0.3120(5) 0.4654(5) 0.072(3) Uani 1 1 d . . . . .
H12 H 0.2587 0.2580 0.4632 0.087 Uiso 1 1 calc R U . . .
C13 C 0.2815(8) 0.3612(6) 0.4255(5) 0.070(3) Uani 1 1 d . . . . .
H13 H 0.3187 0.3408 0.3948 0.084 Uiso 1 1 calc R U . . .
C14 C 0.2648(7) 0.4427(5) 0.4292(4) 0.059(2) Uani 1 1 d . . . . .
H14 H 0.2934 0.4771 0.4024 0.071 Uiso 1 1 calc R U . . .
C15 C 0.1807(7) 0.6288(5) 0.4047(3) 0.051(2) Uani 1 1 d . . . . .
C16 C 0.1457(8) 0.5916(6) 0.3563(4) 0.063(2) Uani 1 1 d . . . . .
H16 H 0.1143 0.5423 0.3590 0.076 Uiso 1 1 calc R U . . .
C17 C 0.1574(9) 0.6282(7) 0.3027(4) 0.078(3) Uani 1 1 d . . . . .
H17 H 0.1339 0.6033 0.2695 0.093 Uiso 1 1 calc R U . . .
C18 C 0.2022(10) 0.6987(8) 0.2992(4) 0.082(3) Uani 1 1 d . . . . .
H18 H 0.2119 0.7220 0.2633 0.098 Uiso 1 1 calc R U . . .
C19 C 0.2329(9) 0.7361(8) 0.3456(4) 0.080(3) Uani 1 1 d . . . . .
H19 H 0.2608 0.7866 0.3423 0.096 Uiso 1 1 calc R U . . .
C20 C 0.2245(8) 0.7021(6) 0.3986(4) 0.061(2) Uani 1 1 d . . . . .
H20 H 0.2487 0.7287 0.4309 0.073 Uiso 1 1 calc R U . . .
C21 C 0.0379(6) 0.5912(4) 0.5094(4) 0.0482(19) Uani 1 1 d . . . . .
C22 C -0.0469(6) 0.5988(5) 0.4755(5) 0.061(2) Uani 1 1 d . . . . .
H22 H -0.0410 0.5993 0.4356 0.073 Uiso 1 1 calc R U . . .
C23 C -0.1408(8) 0.6058(5) 0.5011(5) 0.071(3) Uani 1 1 d . . . . .
H23 H -0.1985 0.6096 0.4781 0.085 Uiso 1 1 calc R U . . .
C24 C -0.1509(8) 0.6072(6) 0.5579(6) 0.072(3) Uani 1 1 d . . . . .
H24 H -0.2147 0.6144 0.5744 0.087 Uiso 1 1 calc R U . . .
C25 C -0.0693(9) 0.5984(5) 0.5912(5) 0.078(3) Uani 1 1 d . . . . .
H25 H -0.0765 0.5966 0.6310 0.094 Uiso 1 1 calc R U . . .
C26 C 0.0259(8) 0.5919(5) 0.5668(5) 0.064(2) Uani 1 1 d . . . . .
H26 H 0.0827 0.5880 0.5905 0.077 Uiso 1 1 calc R U . . .
C27 C 0.4339(6) 0.3927(4) 0.5554(3) 0.0414(17) Uani 1 1 d . . . . .
C28 C 0.4991(6) 0.3651(4) 0.5195(3) 0.0425(16) Uani 1 1 d . . . . .
H28 H 0.5044 0.3101 0.5171 0.051 Uiso 1 1 calc R U . . .
C29 C 0.3146(6) 0.3697(5) 0.6290(3) 0.0458(18) Uani 1 1 d . . . . .
C30 C 0.3194(8) 0.2380(5) 0.6421(4) 0.063(2) Uani 1 1 d . . . . .
H30A H 0.2700 0.2082 0.6199 0.076 Uiso 1 1 calc R U . . .
H30B H 0.3406 0.2062 0.6747 0.076 Uiso 1 1 calc R U . . .
C31 C 0.4096(7) 0.2602(4) 0.6052(3) 0.0489(19) Uani 1 1 d . . . . .
H31 H 0.4080 0.2298 0.5693 0.059 Uiso 1 1 calc R U . . .
C32 C 0.5126(8) 0.2510(6) 0.6335(4) 0.060(2) Uani 1 1 d . . . . .
H32 H 0.5635 0.2694 0.6058 0.073 Uiso 1 1 calc R U . . .
C33 C 0.5214(10) 0.3016(9) 0.6848(5) 0.096(4) Uani 1 1 d . . . . .
H33A H 0.5065 0.3556 0.6746 0.144 Uiso 1 1 calc R U . . .
H33B H 0.4741 0.2840 0.7135 0.144 Uiso 1 1 calc R U . . .
H33C H 0.5893 0.2984 0.6998 0.144 Uiso 1 1 calc R U . . .
C34 C 0.5343(10) 0.1666(7) 0.6454(5) 0.099(4) Uani 1 1 d . . . . .
H34A H 0.5274 0.1365 0.6105 0.148 Uiso 1 1 calc R U . . .
H34B H 0.6023 0.1613 0.6598 0.148 Uiso 1 1 calc R U . . .
H34C H 0.4871 0.1470 0.6736 0.148 Uiso 1 1 calc R U . . .
C35 C 0.5516(6) 0.5347(4) 0.4681(4) 0.0481(18) Uani 1 1 d . . . . .
C36 C 0.5829(7) 0.5843(5) 0.5108(4) 0.062(2) Uani 1 1 d . . . . .
H36 H 0.6192 0.5636 0.5417 0.075 Uiso 1 1 calc R U . . .
C37 C 0.5627(8) 0.6618(6) 0.5094(5) 0.079(3) Uani 1 1 d . . . . .
H37 H 0.5854 0.6947 0.5389 0.094 Uiso 1 1 calc R U . . .
C38 C 0.5087(9) 0.6929(5) 0.4644(7) 0.094(4) Uani 1 1 d . . . . .
H38 H 0.4937 0.7468 0.4635 0.112 Uiso 1 1 calc R U . . .
C39 C 0.4770(8) 0.6449(6) 0.4213(6) 0.081(3) Uani 1 1 d . . . . .
H39 H 0.4403 0.6657 0.3905 0.097 Uiso 1 1 calc R U . . .
C40 C 0.4992(7) 0.5653(5) 0.4233(5) 0.066(3) Uani 1 1 d . . . . .
H40 H 0.4781 0.5323 0.3935 0.079 Uiso 1 1 calc R U . . .
C41 C 0.5831(6) 0.3807(5) 0.3953(3) 0.0496(19) Uani 1 1 d . . . . .
C42 C 0.6239(7) 0.4174(7) 0.3497(4) 0.067(3) Uani 1 1 d . . . . .
H42 H 0.6550 0.4665 0.3545 0.080 Uiso 1 1 calc R U . . .
C43 C 0.6206(11) 0.3840(9) 0.2965(5) 0.093(4) Uani 1 1 d . . . . .
H43 H 0.6486 0.4108 0.2653 0.112 Uiso 1 1 calc R U . . .
C44 C 0.5788(10) 0.3150(10) 0.2890(5) 0.092(4) Uani 1 1 d . . . . .
H44 H 0.5780 0.2926 0.2524 0.110 Uiso 1 1 calc R U . . .
C45 C 0.5376(10) 0.2761(8) 0.3321(5) 0.082(3) Uani 1 1 d . . . . .
H45 H 0.5076 0.2269 0.3258 0.099 Uiso 1 1 calc R U . . .
C46 C 0.5390(8) 0.3075(6) 0.3854(4) 0.061(2) Uani 1 1 d . . . . .
H46 H 0.5099 0.2797 0.4158 0.073 Uiso 1 1 calc R U . . .
C47 C 0.7169(7) 0.4113(4) 0.5054(4) 0.0496(19) Uani 1 1 d . . . . .
C48 C 0.8046(6) 0.4108(5) 0.4737(4) 0.055(2) Uani 1 1 d . . . . .
H48 H 0.8020 0.4169 0.4340 0.066 Uiso 1 1 calc R U . . .
C49 C 0.8966(7) 0.4014(5) 0.5011(5) 0.065(3) Uani 1 1 d . . . . .
H49 H 0.9564 0.4024 0.4797 0.078 Uiso 1 1 calc R U . . .
C50 C 0.9012(8) 0.3909(5) 0.5579(5) 0.068(3) Uani 1 1 d . . . . .
H50 H 0.9638 0.3844 0.5761 0.082 Uiso 1 1 calc R U . . .
C51 C 0.8149(8) 0.3897(5) 0.5887(4) 0.065(3) Uani 1 1 d . . . . .
H51 H 0.8175 0.3810 0.6282 0.078 Uiso 1 1 calc R U . . .
C52 C 0.7248(7) 0.4012(5) 0.5628(4) 0.058(2) Uani 1 1 d . . . . .
H52 H 0.6661 0.4021 0.5851 0.069 Uiso 1 1 calc R U . . .
C53 C 0.3897(15) 1.0318(13) 0.7625(6) 0.169(10) Uani 1 1 d D . . . .
H53A H 0.3873 1.0890 0.7581 0.203 Uiso 1 1 calc R U . . .
H53B H 0.4525 1.0188 0.7822 0.203 Uiso 1 1 calc R U . . .
C54A C 0.1117(12) 0.4447(13) 0.7338(7) 0.176(10) Uani 0.4 1 d D . P A 1
H54A H 0.1454 0.3977 0.7484 0.211 Uiso 0.4 1 calc R U P A 1
H54B H 0.1380 0.4557 0.6957 0.211 Uiso 0.4 1 calc R U P A 1
C54B C 0.1117(12) 0.4447(13) 0.7338(7) 0.176(10) Uani 0.4 1 d D . P B 2
H54C H 0.1733 0.4306 0.7133 0.211 Uiso 0.4 1 calc R U P B 2
H54D H 0.0917 0.3995 0.7570 0.211 Uiso 0.4 1 calc R U P B 2
C54C C 0.1117(12) 0.4447(13) 0.7338(7) 0.176(10) Uani 0.2 1 d D . P C 3
H54E H 0.1728 0.4165 0.7226 0.211 Uiso 0.2 1 calc R U P C 3
H54F H 0.0736 0.4602 0.6999 0.211 Uiso 0.2 1 calc R U P C 3
 
 
_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 C2 1.907(8) . ?
Ge1 C15 1.939(8) . ?
Ge1 C9 1.954(7) . ?
Ge1 C21 1.962(8) . ?
Ge2 C28 1.913(8) . ?
Ge2 C41 1.952(8) . ?
Ge2 C35 1.955(7) . ?
Ge2 C47 1.963(9) . ?
Zn1 C1 1.989(8) . ?
Zn1 C27 2.008(8) . ?
Zn1 O3 2.249(6) . ?
Zn1 O1 2.257(6) . ?
Cl1 C53 1.679(16) . ?
Cl2 C53 1.731(16) . ?
Cl3A C54A 1.707(17) . ?
Cl4A C54A 1.744(17) . ?
Cl3B C54B 1.707(17) . ?
Cl4B C54B 1.671(18) . ?
Cl3C C54C 1.707(17) . ?
Cl4C C54C 1.72(2) . ?
O1 C3 1.210(11) . ?
O2 C3 1.367(10) . ?
O2 C4 1.448(12) . ?
O3 C29 1.195(11) . ?
O4 C29 1.356(10) . ?
O4 C30 1.446(11) . ?
N1 C3 1.334(12) . ?
N1 C1 1.424(10) . ?
N1 C5 1.475(11) . ?
N2 C29 1.363(10) . ?
N2 C27 1.416(10) . ?
N2 C31 1.465(9) . ?
C1 C2 1.333(11) . ?
C4 C5 1.542(13) . ?
C5 C6 1.517(15) . ?
C6 C7 1.501(19) . ?
C6 C8 1.533(17) . ?
C9 C14 1.392(12) . ?
C9 C10 1.399(12) . ?
C10 C11 1.373(12) . ?
C11 C12 1.365(15) . ?
C12 C13 1.362(15) . ?
C13 C14 1.422(13) . ?
C15 C16 1.397(12) . ?
C15 C20 1.398(13) . ?
C16 C17 1.427(14) . ?
C17 C18 1.356(17) . ?
C18 C19 1.341(17) . ?
C19 C20 1.392(13) . ?
C21 C26 1.371(14) . ?
C21 C22 1.400(13) . ?
C22 C23 1.405(14) . ?
C23 C24 1.356(15) . ?
C24 C25 1.359(17) . ?
C25 C26 1.407(14) . ?
C27 C28 1.312(11) . ?
C30 C31 1.542(13) . ?
C31 C32 1.545(13) . ?
C32 C33 1.501(14) . ?
C32 C34 1.509(14) . ?
C35 C40 1.380(13) . ?
C35 C36 1.389(12) . ?
C36 C37 1.362(13) . ?
C37 C38 1.397(18) . ?
C38 C39 1.382(17) . ?
C39 C40 1.403(13) . ?
C41 C42 1.366(12) . ?
C41 C46 1.412(13) . ?
C42 C43 1.386(16) . ?
C43 C44 1.327(19) . ?
C44 C45 1.342(18) . ?
C45 C46 1.375(14) . ?
C47 C52 1.377(13) . ?
C47 C48 1.396(12) . ?
C48 C49 1.406(13) . ?
C49 C50 1.361(14) . ?
C50 C51 1.370(16) . ?
C51 C52 1.372(14) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
C2 Ge1 C15 109.0(4) . . ?
C2 Ge1 C9 114.2(3) . . ?
C15 Ge1 C9 109.6(3) . . ?
C2 Ge1 C21 104.7(3) . . ?
C15 Ge1 C21 110.5(4) . . ?
C9 Ge1 C21 108.7(3) . . ?
C28 Ge2 C41 110.0(3) . . ?
C28 Ge2 C35 113.8(3) . . ?
C41 Ge2 C35 109.5(3) . . ?
C28 Ge2 C47 103.8(3) . . ?
C41 Ge2 C47 110.3(3) . . ?
C35 Ge2 C47 109.3(3) . . ?
C1 Zn1 C27 165.6(3) . . ?
C1 Zn1 O3 107.7(3) . . ?
C27 Zn1 O3 82.6(3) . . ?
C1 Zn1 O1 82.1(3) . . ?
C27 Zn1 O1 108.3(3) . . ?
O3 Zn1 O1 91.3(3) . . ?
C3 O1 Zn1 102.6(6) . . ?
C3 O2 C4 108.5(7) . . ?
C29 O3 Zn1 102.8(5) . . ?
C29 O4 C30 109.4(6) . . ?
C3 N1 C1 119.5(7) . . ?
C3 N1 C5 112.4(7) . . ?
C1 N1 C5 127.8(7) . . ?
C29 N2 C27 119.6(7) . . ?
C29 N2 C31 112.0(6) . . ?
C27 N2 C31 128.1(7) . . ?
C2 C1 N1 119.4(7) . . ?
C2 C1 Zn1 132.8(6) . . ?
N1 C1 Zn1 107.8(5) . . ?
C1 C2 Ge1 124.9(5) . . ?
O1 C3 N1 128.0(9) . . ?
O1 C3 O2 121.6(9) . . ?
N1 C3 O2 110.4(8) . . ?
O2 C4 C5 105.5(7) . . ?
N1 C5 C6 113.3(8) . . ?
N1 C5 C4 99.1(7) . . ?
C6 C5 C4 115.7(9) . . ?
C7 C6 C5 112.0(11) . . ?
C7 C6 C8 113.2(12) . . ?
C5 C6 C8 108.6(11) . . ?
C14 C9 C10 118.7(8) . . ?
C14 C9 Ge1 121.2(7) . . ?
C10 C9 Ge1 120.0(6) . . ?
C11 C10 C9 121.2(9) . . ?
C12 C11 C10 120.4(9) . . ?
C13 C12 C11 120.2(9) . . ?
C12 C13 C14 120.8(10) . . ?
C9 C14 C13 118.6(10) . . ?
C16 C15 C20 118.1(9) . . ?
C16 C15 Ge1 122.1(7) . . ?
C20 C15 Ge1 119.8(7) . . ?
C15 C16 C17 119.5(10) . . ?
C18 C17 C16 119.9(10) . . ?
C19 C18 C17 121.0(11) . . ?
C18 C19 C20 121.0(12) . . ?
C19 C20 C15 120.4(10) . . ?
C26 C21 C22 118.3(9) . . ?
C26 C21 Ge1 118.6(7) . . ?
C22 C21 Ge1 123.0(7) . . ?
C21 C22 C23 119.3(10) . . ?
C24 C23 C22 121.4(11) . . ?
C23 C24 C25 119.7(11) . . ?
C24 C25 C26 120.2(11) . . ?
C21 C26 C25 121.1(11) . . ?
C28 C27 N2 119.6(7) . . ?
C28 C27 Zn1 133.6(6) . . ?
N2 C27 Zn1 106.8(5) . . ?
C27 C28 Ge2 126.6(6) . . ?
O3 C29 O4 122.1(7) . . ?
O3 C29 N2 128.1(8) . . ?
O4 C29 N2 109.8(7) . . ?
O4 C30 C31 105.5(7) . . ?
N2 C31 C30 100.0(7) . . ?
N2 C31 C32 111.8(7) . . ?
C30 C31 C32 115.6(7) . . ?
C33 C32 C34 113.1(10) . . ?
C33 C32 C31 111.3(8) . . ?
C34 C32 C31 110.6(10) . . ?
C40 C35 C36 118.7(8) . . ?
C40 C35 Ge2 121.2(7) . . ?
C36 C35 Ge2 120.1(6) . . ?
C37 C36 C35 121.7(10) . . ?
C36 C37 C38 119.8(11) . . ?
C39 C38 C37 119.8(9) . . ?
C38 C39 C40 119.5(11) . . ?
C35 C40 C39 120.5(11) . . ?
C42 C41 C46 116.6(9) . . ?
C42 C41 Ge2 123.4(8) . . ?
C46 C41 Ge2 120.0(7) . . ?
C41 C42 C43 121.1(11) . . ?
C44 C43 C42 120.5(11) . . ?
C43 C44 C45 121.2(12) . . ?
C44 C45 C46 120.0(13) . . ?
C45 C46 C41 120.7(10) . . ?
C52 C47 C48 117.8(9) . . ?
C52 C47 Ge2 119.4(7) . . ?
C48 C47 Ge2 122.8(7) . . ?
C47 C48 C49 119.6(9) . . ?
C50 C49 C48 120.9(10) . . ?
C49 C50 C51 119.4(10) . . ?
C50 C51 C52 120.3(10) . . ?
C51 C52 C47 122.0(10) . . ?
Cl1 C53 Cl2 115.0(10) . . ?
Cl3A C54A Cl4A 110.4(11) . . ?
Cl4B C54B Cl3B 113.0(14) . . ?
Cl3C C54C Cl4C 96.5(12) . . ?



################################################################################

data_Compound_58
 
_audit_creation_method            'SHELXL-2017/1'
_shelx_SHELXL_version_number      '2017/1'
_chemical_formula_moiety          'C32 H35 Ge O3 P'
_chemical_formula_sum             'C32 H35 Ge O3 P'
_chemical_formula_weight          571.16

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'
 'O'  'O'   0.0106   0.0060
 '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'
 
_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                    16.3298(9)
_cell_length_b                    12.8553(7)
_cell_length_c                    28.1785(16)
_cell_angle_alpha                 90
_cell_angle_beta                  97.582(2)
_cell_angle_gamma                 90
_cell_volume                      5863.6(6)
_cell_formula_units_Z             8
_cell_measurement_temperature     200(1)
_cell_measurement_reflns_used     9957
_cell_measurement_theta_min       2.21
_cell_measurement_theta_max       30.49
 
_exptl_crystal_description        'fragment'
_exptl_crystal_colour             'colourless'
_exptl_crystal_size_max           0.25
_exptl_crystal_size_mid           0.2
_exptl_crystal_size_min           0.15
_exptl_crystal_density_method     'not measured'
_exptl_crystal_density_diffrn     1.294          
_exptl_crystal_F_000              2384
_exptl_absorpt_coefficient_mu     1.129
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.699
_exptl_absorpt_correction_T_max   0.746
_exptl_absorpt_process_details     
; 
 SADABS : Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
; 
 
_diffrn_ambient_temperature       200(1)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   'curved graphite'
_diffrn_measurement_device_type   'Bruker APEX-II CCD'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_reflns_number             34893
_diffrn_reflns_av_unetI/netI      0.0168
_diffrn_reflns_av_R_equivalents   0.0179
_diffrn_reflns_limit_h_min        -23
_diffrn_reflns_limit_h_max        22
_diffrn_reflns_limit_k_min        -18
_diffrn_reflns_limit_k_max        18
_diffrn_reflns_limit_l_min        -40
_diffrn_reflns_limit_l_max        40
_diffrn_reflns_theta_min          2.206
_diffrn_reflns_theta_max          30.545
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.998
_diffrn_measured_fraction_theta_full  0.999
_diffrn_reflns_Laue_measured_fraction_max    0.998
_diffrn_reflns_Laue_measured_fraction_full   0.999
_diffrn_reflns_point_group_measured_fraction_max   0.998
_diffrn_reflns_point_group_measured_fraction_full  0.999
_reflns_number_total              8973
_reflns_number_gt                 7907
_reflns_threshold_expression      'I > 2σ(I)'
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;
 
_computing_data_collection        'Bruker APEX2'
_computing_cell_refinement        'Bruker SAINT'
_computing_data_reduction         'Bruker SAINT'
_computing_structure_solution     'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement   'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics     'SXGRAPH (Farrugia, 2012)'
_computing_publication_material   'WinGX (Farrugia, 2012)'

_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0296P)²+4.7258P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      dual
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_number_reflns          8973
_refine_ls_number_parameters      334
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0338
_refine_ls_R_factor_gt            0.0273
_refine_ls_wR_factor_ref          0.0683
_refine_ls_wR_factor_gt           0.0653
_refine_ls_goodness_of_fit_ref    1.050
_refine_ls_restrained_S_all       1.050
_refine_ls_shift/su_max           0.002
_refine_ls_shift/su_mean          0.000
_refine_diff_density_max          0.376
_refine_diff_density_min         -0.285
_refine_diff_density_rms          0.047
 
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 0.75803(2) 0.53687(2) 0.42991(2) 0.02043(4) Uani 1 1 d . . . . .
P1 P 0.73600(2) 0.71732(3) 0.28920(2) 0.02349(7) Uani 1 1 d . . . . .
O1 O 0.69721(6) 0.82185(7) 0.30518(3) 0.02948(19) Uani 1 1 d . . . . .
O2 O 0.82568(6) 0.74488(8) 0.27755(3) 0.0301(2) Uani 1 1 d . . . . .
O3 O 0.68918(6) 0.66403(8) 0.24834(3) 0.0333(2) Uani 1 1 d . . . . .
C1 C 0.70644(7) 0.62588(9) 0.37728(4) 0.0210(2) Uani 1 1 d . . . . .
C2 C 0.75593(7) 0.64516(10) 0.34382(4) 0.0238(2) Uani 1 1 d . . . . .
H2 H 0.809740 0.616047 0.350118 0.029 Uiso 1 1 calc R U . . .
C3 C 0.71140(8) 0.54512(10) 0.49000(4) 0.0236(2) Uani 1 1 d . . . . .
C4 C 0.63379(8) 0.50194(12) 0.49315(5) 0.0317(3) Uani 1 1 d . . . . .
H4 H 0.602232 0.474277 0.465261 0.038 Uiso 1 1 calc R U . . .
C5 C 0.60210(10) 0.49894(14) 0.53667(6) 0.0398(3) Uani 1 1 d . . . . .
H5 H 0.549280 0.469250 0.538321 0.048 Uiso 1 1 calc R U . . .
C6 C 0.64721(12) 0.53891(13) 0.57723(5) 0.0434(4) Uani 1 1 d . . . . .
H6 H 0.625443 0.536523 0.606859 0.052 Uiso 1 1 calc R U . . .
C7 C 0.72405(11) 0.58257(12) 0.57516(5) 0.0392(3) Uani 1 1 d . . . . .
H7 H 0.754877 0.610574 0.603204 0.047 Uiso 1 1 calc R U . . .
C8 C 0.75606(9) 0.58526(11) 0.53162(5) 0.0295(3) Uani 1 1 d . . . . .
H8 H 0.809024 0.614846 0.530302 0.035 Uiso 1 1 calc R U . . .
C9 C 0.87459(7) 0.57463(11) 0.43934(4) 0.0255(2) Uani 1 1 d . . . . .
C10 C 0.93474(9) 0.50382(14) 0.42963(6) 0.0392(3) Uani 1 1 d . . . . .
H10 H 0.919307 0.435104 0.419780 0.047 Uiso 1 1 calc R U . . .
C11 C 1.01755(10) 0.53347(19) 0.43432(7) 0.0557(5) Uani 1 1 d . . . . .
H11 H 1.058254 0.484790 0.427604 0.067 Uiso 1 1 calc R U . . .
C12 C 1.04061(10) 0.6322(2) 0.44853(6) 0.0589(6) Uani 1 1 d . . . . .
H12 H 1.097226 0.651603 0.451941 0.071 Uiso 1 1 calc R U . . .
C13 C 0.98186(11) 0.70361(17) 0.45791(6) 0.0512(4) Uani 1 1 d . . . . .
H13 H 0.997925 0.772285 0.467485 0.061 Uiso 1 1 calc R U . . .
C14 C 0.89889(9) 0.67503(12) 0.45333(5) 0.0358(3) Uani 1 1 d . . . . .
H14 H 0.858579 0.724472 0.459815 0.043 Uiso 1 1 calc R U . . .
C15 C 0.74264(7) 0.39387(10) 0.40793(4) 0.0227(2) Uani 1 1 d . . . . .
C16 C 0.70926(9) 0.36877(11) 0.36114(5) 0.0314(3) Uani 1 1 d . . . . .
H16 H 0.692278 0.422791 0.339003 0.038 Uiso 1 1 calc R U . . .
C17 C 0.70063(10) 0.26562(13) 0.34661(5) 0.0379(3) Uani 1 1 d . . . . .
H17 H 0.678075 0.249552 0.314638 0.046 Uiso 1 1 calc R U . . .
C18 C 0.72466(9) 0.18668(11) 0.37839(5) 0.0354(3) Uani 1 1 d . . . . .
H18 H 0.719127 0.116271 0.368240 0.042 Uiso 1 1 calc R U . . .
C19 C 0.75686(9) 0.20967(11) 0.42508(5) 0.0330(3) Uani 1 1 d . . . . .
H19 H 0.772881 0.155098 0.447095 0.040 Uiso 1 1 calc R U . . .
C20 C 0.76573(8) 0.31255(11) 0.43973(4) 0.0289(3) Uani 1 1 d . . . . .
H20 H 0.787837 0.327873 0.471854 0.035 Uiso 1 1 calc R U . . .
C21 C 0.61849(7) 0.65722(9) 0.37350(4) 0.0223(2) Uani 1 1 d . . . . .
C22 C 0.56415(8) 0.63865(11) 0.33164(5) 0.0300(3) Uani 1 1 d . . . . .
H22 H 0.583668 0.605640 0.305126 0.036 Uiso 1 1 calc R U . . .
C23 C 0.48149(9) 0.66838(13) 0.32866(6) 0.0413(4) Uani 1 1 d . . . . .
H23 H 0.445064 0.655880 0.300066 0.050 Uiso 1 1 calc R U . . .
C24 C 0.45237(9) 0.71580(14) 0.36700(7) 0.0471(4) Uani 1 1 d . . . . .
H24 H 0.396145 0.736557 0.364655 0.057 Uiso 1 1 calc R U . . .
C25 C 0.50495(10) 0.73318(13) 0.40886(6) 0.0421(4) Uani 1 1 d . . . . .
H25 H 0.484678 0.765406 0.435324 0.050 Uiso 1 1 calc R U . . .
C26 C 0.58758(8) 0.70354(11) 0.41233(5) 0.0295(3) Uani 1 1 d . . . . .
H26 H 0.623214 0.714914 0.441338 0.035 Uiso 1 1 calc R U . . .
C27 C 0.62891(8) 0.87540(11) 0.27593(5) 0.0325(3) Uani 1 1 d . . . . .
H27 H 0.589620 0.822294 0.260153 0.039 Uiso 1 1 calc R U . . .
C28 C 0.58616(11) 0.93731(15) 0.31068(7) 0.0520(4) Uani 1 1 d . . . . .
H28A H 0.539523 0.975223 0.293233 0.078 Uiso 1 1 calc R U . . .
H28B H 0.565874 0.890157 0.333851 0.078 Uiso 1 1 calc R U . . .
H28C H 0.625200 0.986902 0.327617 0.078 Uiso 1 1 calc R U . . .
C29 C 0.66206(13) 0.9389(2) 0.23797(9) 0.0728(7) Uani 1 1 d . . . . .
H29A H 0.616334 0.974541 0.218502 0.109 Uiso 1 1 calc R U . . .
H29B H 0.701262 0.990494 0.253145 0.109 Uiso 1 1 calc R U . . .
H29C H 0.690198 0.893084 0.217512 0.109 Uiso 1 1 calc R U . . .
C30 C 0.88586(9) 0.80020(14) 0.31128(5) 0.0381(3) Uani 1 1 d . . . . .
H30 H 0.862422 0.811415 0.341924 0.046 Uiso 1 1 calc R U . . .
C31 C 0.90163(13) 0.90374(16) 0.28948(9) 0.0611(5) Uani 1 1 d . . . . .
H31A H 0.941964 0.942804 0.311403 0.092 Uiso 1 1 calc R U . . .
H31B H 0.923360 0.892920 0.259056 0.092 Uiso 1 1 calc R U . . .
H31C H 0.849840 0.943041 0.283748 0.092 Uiso 1 1 calc R U . . .
C32 C 0.96215(11) 0.73344(19) 0.32073(7) 0.0578(5) Uani 1 1 d . . . . .
H32A H 1.003623 0.769014 0.343351 0.087 Uiso 1 1 calc R U . . .
H32B H 0.947857 0.666746 0.334348 0.087 Uiso 1 1 calc R U . . .
H32C H 0.984559 0.721145 0.290624 0.087 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 C15 1.9455(13) . ?
Ge1 C9 1.9482(12) . ?
Ge1 C3 1.9489(12) . ?
Ge1 C1 1.9719(11) . ?
P1 O3 1.4653(10) . ?
P1 O1 1.5765(10) . ?
P1 O2 1.5825(10) . ?
P1 C2 1.7898(12) . ?
O1 C27 1.4678(15) . ?
O2 C30 1.4589(17) . ?
C1 C2 1.3434(16) . ?
C1 C21 1.4819(16) . ?
C3 C8 1.3957(18) . ?
C3 C4 1.3972(19) . ?
C4 C5 1.3930(19) . ?
C5 C6 1.375(2) . ?
C6 C7 1.383(3) . ?
C7 C8 1.3961(19) . ?
C9 C14 1.392(2) . ?
C9 C10 1.3925(19) . ?
C10 C11 1.394(2) . ?
C11 C12 1.369(3) . ?
C12 C13 1.378(3) . ?
C13 C14 1.393(2) . ?
C15 C20 1.3959(17) . ?
C15 C16 1.3966(17) . ?
C16 C17 1.389(2) . ?
C17 C18 1.376(2) . ?
C18 C19 1.383(2) . ?
C19 C20 1.387(2) . ?
C21 C26 1.3973(18) . ?
C21 C22 1.3999(17) . ?
C22 C23 1.395(2) . ?
C23 C24 1.379(3) . ?
C24 C25 1.382(3) . ?
C25 C26 1.3932(19) . ?
C27 C29 1.502(2) . ?
C27 C28 1.504(2) . ?
C30 C31 1.502(3) . ?
C30 C32 1.507(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
C15 Ge1 C9 111.20(5) . . ?
C15 Ge1 C3 106.21(5) . . ?
C9 Ge1 C3 110.77(5) . . ?
C15 Ge1 C1 106.53(5) . . ?
C9 Ge1 C1 105.71(5) . . ?
C3 Ge1 C1 116.40(5) . . ?
O3 P1 O1 115.81(6) . . ?
O3 P1 O2 110.05(6) . . ?
O1 P1 O2 106.63(6) . . ?
O3 P1 C2 116.76(6) . . ?
O1 P1 C2 103.32(5) . . ?
O2 P1 C2 103.07(5) . . ?
C27 O1 P1 122.92(9) . . ?
C30 O2 P1 122.43(8) . . ?
C2 C1 C21 124.50(10) . . ?
C2 C1 Ge1 113.45(8) . . ?
C21 C1 Ge1 121.72(8) . . ?
C1 C2 P1 129.89(9) . . ?
C8 C3 C4 118.13(12) . . ?
C8 C3 Ge1 121.97(10) . . ?
C4 C3 Ge1 119.68(10) . . ?
C5 C4 C3 120.81(14) . . ?
C6 C5 C4 120.07(15) . . ?
C5 C6 C7 120.40(13) . . ?
C6 C7 C8 119.62(14) . . ?
C3 C8 C7 120.97(14) . . ?
C14 C9 C10 118.66(13) . . ?
C14 C9 Ge1 120.44(10) . . ?
C10 C9 Ge1 120.81(11) . . ?
C9 C10 C11 120.21(17) . . ?
C12 C11 C10 120.47(17) . . ?
C11 C12 C13 120.13(15) . . ?
C12 C13 C14 119.99(18) . . ?
C9 C14 C13 120.54(16) . . ?
C20 C15 C16 118.14(12) . . ?
C20 C15 Ge1 119.39(9) . . ?
C16 C15 Ge1 122.47(9) . . ?
C17 C16 C15 120.69(13) . . ?
C18 C17 C16 120.20(13) . . ?
C17 C18 C19 120.11(13) . . ?
C18 C19 C20 119.89(13) . . ?
C19 C20 C15 120.95(12) . . ?
C26 C21 C22 118.58(11) . . ?
C26 C21 C1 120.41(11) . . ?
C22 C21 C1 120.99(11) . . ?
C23 C22 C21 120.31(14) . . ?
C24 C23 C22 120.35(14) . . ?
C23 C24 C25 120.03(13) . . ?
C24 C25 C26 120.17(15) . . ?
C25 C26 C21 120.54(13) . . ?
O1 C27 C29 109.66(13) . . ?
O1 C27 C28 105.43(12) . . ?
C29 C27 C28 114.71(16) . . ?
O2 C30 C31 107.61(14) . . ?
O2 C30 C32 107.91(14) . . ?
C31 C30 C32 113.23(15) . . ?



################################################################################


