#------------------------------------------------------------------------------
#$Date: 2024-01-06 09:23:42 +0200 (Sat, 06 Jan 2024) $
#$Revision: 288746 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/03/1570323.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1570323
loop_
_publ_author_name
'Peddi, Balakrishna'
'Khan, Souvik'
'Gonnade, Rajesh G.'
'Yildiz, Cem B.'
'Majumdar, Moumita'
_publ_section_title
;
 Intramolecular donor-stabilized tetra-coordinated germanium(iv)
 di-cations and their Lewis acidic properties.
;
_journal_issue                   47
_journal_name_full               'Chemical science'
_journal_page_first              13755
_journal_page_last               13764
_journal_paper_doi               10.1039/d3sc03717g
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C43 H54 Ge N2 P2, 2(C F3 S O3), 2(C H2 Cl2)'
_chemical_formula_sum            'C47 H58 Cl4 F6 Ge N2 O6 P2 S2'
_chemical_formula_weight         1201.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-12-02 deposited with the CCDC.	2023-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.04(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.282(11)
_cell_length_b                   30.08(3)
_cell_length_c                   15.527(16)
_cell_measurement_reflns_used    458
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      17.38
_cell_measurement_theta_min      2.43
_cell_volume                     5153(9)
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL, Mercury 2020.20'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1208
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            114081
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.966
_diffrn_source                   'micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.017
_exptl_absorpt_correction_T_max  0.0949
_exptl_absorpt_correction_T_min  0.0686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (BRUKER, 2016)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_description       block
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.329
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.113
_refine_diff_density_max         3.111
_refine_diff_density_min         -2.112
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         9588
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1293
_refine_ls_R_factor_gt           0.0933
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0959P)²+66.1282P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2238
_refine_ls_wR_factor_ref         0.2506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6932
_reflns_number_total             9588
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3sc03717g2.cif
_cod_data_source_block           mo_BA_203small_0m
_cod_depositor_comments
'Adding full bibliography for 1570312--1570327.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1570323
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_min   0.731
_shelx_estimated_absorpt_t_max   0.894
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'
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 0.89547(7) 0.64366(2) 0.20573(5) 0.0184(2) Uani 1 1 d . . . . .
C1 C 0.9788(6) 0.5995(2) 0.1479(4) 0.0203(15) Uani 1 1 d . . . . .
P1 P 1.07024(16) 0.70213(6) 0.23560(12) 0.0186(4) Uani 1 1 d . . . . .
P2 P 0.72098(17) 0.58582(6) 0.17491(12) 0.0214(4) Uani 1 1 d . . . . .
C2 C 0.7942(7) 0.6969(2) 0.1949(5) 0.0222(15) Uani 1 1 d . . . . .
N1 N 0.9317(5) 0.62635(18) 0.3305(4) 0.0157(12) Uani 1 1 d . . . . .
N2 N 1.0123(6) 0.5883(2) 0.5881(4) 0.0308(15) Uani 1 1 d . . . . .
C3 C 1.0890(6) 0.6070(2) 0.1275(4) 0.0206(15) Uani 1 1 d . . . . .
H3 H 1.1183 0.6367 0.1289 0.025 Uiso 1 1 calc R U . . .
C4 C 1.1608(7) 0.5727(2) 0.1043(5) 0.0255(16) Uani 1 1 d . . . . .
H4 H 1.2353 0.5793 0.0877 0.031 Uiso 1 1 calc R U . . .
C5 C 1.1223(6) 0.5295(2) 0.1060(4) 0.0224(15) Uani 1 1 d . . . . .
C6 C 0.9821(7) 0.4766(2) 0.1257(5) 0.0256(17) Uani 1 1 d . . . . .
C7 C 0.8734(7) 0.4638(3) 0.1427(5) 0.0287(17) Uani 1 1 d . . . . .
H7 H 0.8523 0.4332 0.1426 0.034 Uiso 1 1 calc R U . . .
C8 C 0.7939(7) 0.4963(2) 0.1600(5) 0.0262(16) Uani 1 1 d . . . . .
H8 H 0.7181 0.4873 0.1716 0.031 Uiso 1 1 calc R U . . .
C9 C 0.8204(7) 0.5413(2) 0.1611(5) 0.0232(16) Uani 1 1 d . . . . .
C10 C 1.0107(7) 0.5218(2) 0.1262(5) 0.0214(15) Uani 1 1 d . . . . .
C11 C 0.9333(6) 0.5554(2) 0.1446(4) 0.0191(15) Uani 1 1 d . . . . .
C12 C 1.1795(7) 0.4859(2) 0.0901(5) 0.0275(17) Uani 1 1 d . . . . .
H12A H 1.2589 0.4822 0.1309 0.033 Uiso 1 1 calc R U . . .
H12B H 1.1913 0.4840 0.0287 0.033 Uiso 1 1 calc R U . . .
C13 C 1.0880(7) 0.4503(3) 0.1075(5) 0.0307(18) Uani 1 1 d . . . . .
H13A H 1.0625 0.4309 0.0554 0.037 Uiso 1 1 calc R U . . .
H13B H 1.1241 0.4316 0.1587 0.037 Uiso 1 1 calc R U . . .
C14 C 0.6700(7) 0.6957(3) 0.1649(5) 0.0270(17) Uani 1 1 d . . . . .
H14 H 0.6335 0.6688 0.1406 0.032 Uiso 1 1 calc R U . . .
C15 C 0.5958(7) 0.7329(3) 0.1691(6) 0.037(2) Uani 1 1 d . . . . .
H15 H 0.5111 0.7313 0.1455 0.044 Uiso 1 1 calc R U . . .
C16 C 0.6465(7) 0.7711(3) 0.2072(6) 0.036(2) Uani 1 1 d . . . . .
C17 C 0.8106(7) 0.8127(2) 0.2805(5) 0.0284(17) Uani 1 1 d . . . . .
C18 C 0.9296(7) 0.8174(2) 0.3179(5) 0.0274(17) Uani 1 1 d . . . . .
H18 H 0.9573 0.8435 0.3502 0.033 Uiso 1 1 calc R U . . .
C19 C 1.0120(7) 0.7835(2) 0.3086(5) 0.0239(16) Uani 1 1 d . . . . .
H19 H 1.0957 0.7876 0.3332 0.029 Uiso 1 1 calc R U . . .
C20 C 0.9741(6) 0.7444(2) 0.2644(5) 0.0203(15) Uani 1 1 d . . . . .
C21 C 0.7721(7) 0.7724(2) 0.2387(5) 0.0257(16) Uani 1 1 d . . . . .
C22 C 0.8489(7) 0.7371(2) 0.2315(5) 0.0221(15) Uani 1 1 d . . . . .
C23 C 0.7029(8) 0.8431(3) 0.2743(6) 0.038(2) Uani 1 1 d . . . . .
H23A H 0.7121 0.8700 0.2397 0.045 Uiso 1 1 calc R U . . .
H23B H 0.6926 0.8521 0.3336 0.045 Uiso 1 1 calc R U . . .
C24 C 0.5938(9) 0.8148(3) 0.2271(8) 0.049(3) Uani 1 1 d . . . . .
H24A H 0.5351 0.8105 0.2656 0.059 Uiso 1 1 calc R U . . .
H24B H 0.5520 0.8295 0.1721 0.059 Uiso 1 1 calc R U . . .
C25 C 1.2084(6) 0.7003(2) 0.3208(5) 0.0231(16) Uani 1 1 d . . . . .
H25 H 1.2430 0.7311 0.3274 0.028 Uiso 1 1 calc R U . . .
C26 C 1.1835(7) 0.6863(3) 0.4094(5) 0.0286(17) Uani 1 1 d . . . . .
H26A H 1.1157 0.7038 0.4221 0.043 Uiso 1 1 calc R U . . .
H26B H 1.2559 0.6916 0.4555 0.043 Uiso 1 1 calc R U . . .
H26C H 1.1629 0.6547 0.4078 0.043 Uiso 1 1 calc R U . . .
C27 C 1.3019(7) 0.6700(3) 0.2936(6) 0.0345(19) Uani 1 1 d . . . . .
H27A H 1.2700 0.6397 0.2861 0.052 Uiso 1 1 calc R U . . .
H27B H 1.3764 0.6704 0.3393 0.052 Uiso 1 1 calc R U . . .
H27C H 1.3197 0.6806 0.2379 0.052 Uiso 1 1 calc R U . . .
C28 C 1.1167(7) 0.7245(2) 0.1376(5) 0.0261(17) Uani 1 1 d . . . . .
H28 H 1.1737 0.7024 0.1202 0.031 Uiso 1 1 calc R U . . .
C29 C 1.1849(8) 0.7685(2) 0.1539(5) 0.0311(18) Uani 1 1 d . . . . .
H29A H 1.2082 0.7783 0.0995 0.047 Uiso 1 1 calc R U . . .
H29B H 1.2577 0.7646 0.2002 0.047 Uiso 1 1 calc R U . . .
H29C H 1.1324 0.7910 0.1724 0.047 Uiso 1 1 calc R U . . .
C30 C 1.0091(8) 0.7280(3) 0.0615(5) 0.038(2) Uani 1 1 d . . . . .
H30A H 1.0357 0.7395 0.0096 0.056 Uiso 1 1 calc R U . . .
H30B H 0.9488 0.7482 0.0772 0.056 Uiso 1 1 calc R U . . .
H30C H 0.9729 0.6985 0.0482 0.056 Uiso 1 1 calc R U . . .
C31 C 0.6172(7) 0.5910(2) 0.0662(5) 0.0249(16) Uani 1 1 d . . . . .
H31 H 0.5531 0.6131 0.0720 0.030 Uiso 1 1 calc R U . . .
C32 C 0.6864(8) 0.6093(3) 0.0007(5) 0.0314(18) Uani 1 1 d . . . . .
H32A H 0.6337 0.6097 -0.0581 0.047 Uiso 1 1 calc R U . . .
H32B H 0.7571 0.5905 0.0000 0.047 Uiso 1 1 calc R U . . .
H32C H 0.7133 0.6396 0.0176 0.047 Uiso 1 1 calc R U . . .
C33 C 0.5544(8) 0.5473(3) 0.0345(6) 0.036(2) Uani 1 1 d . . . . .
H33A H 0.4972 0.5521 -0.0216 0.054 Uiso 1 1 calc R U . . .
H33B H 0.5105 0.5363 0.0784 0.054 Uiso 1 1 calc R U . . .
H33C H 0.6152 0.5253 0.0262 0.054 Uiso 1 1 calc R U . . .
C34 C 0.6276(7) 0.5681(3) 0.2525(5) 0.0266(16) Uani 1 1 d . . . . .
H34 H 0.5758 0.5429 0.2247 0.032 Uiso 1 1 calc R U . . .
C35 C 0.5437(8) 0.6059(3) 0.2650(6) 0.042(2) Uani 1 1 d . . . . .
H35A H 0.4919 0.6136 0.2081 0.063 Uiso 1 1 calc R U . . .
H35B H 0.5919 0.6318 0.2890 0.063 Uiso 1 1 calc R U . . .
H35C H 0.4930 0.5966 0.3059 0.063 Uiso 1 1 calc R U . . .
C36 C 0.7019(7) 0.5518(3) 0.3381(5) 0.0326(19) Uani 1 1 d . . . . .
H36A H 0.7603 0.5296 0.3264 0.049 Uiso 1 1 calc R U . . .
H36B H 0.6485 0.5381 0.3730 0.049 Uiso 1 1 calc R U . . .
H36C H 0.7454 0.5768 0.3707 0.049 Uiso 1 1 calc R U . . .
C37 C 0.8895(7) 0.6495(3) 0.3880(5) 0.0290(17) Uani 1 1 d . . . . .
H37 H 0.8411 0.6749 0.3688 0.035 Uiso 1 1 calc R U . . .
C38 C 0.9126(7) 0.6384(3) 0.4750(5) 0.0301(18) Uani 1 1 d . . . . .
H38 H 0.8804 0.6557 0.5159 0.036 Uiso 1 1 calc R U . . .
C39 C 0.9856(7) 0.6005(3) 0.5039(5) 0.0286(17) Uani 1 1 d . . . . .
C40 C 1.0293(7) 0.5767(3) 0.4391(5) 0.0279(17) Uani 1 1 d . . . . .
H40 H 1.0786 0.5512 0.4548 0.033 Uiso 1 1 calc R U . . .
C41 C 1.0007(7) 0.5906(3) 0.3538(5) 0.0250(16) Uani 1 1 d . . . . .
H41 H 1.0303 0.5744 0.3101 0.030 Uiso 1 1 calc R U . . .
C42 C 0.9728(8) 0.6141(3) 0.6556(5) 0.035(2) Uani 1 1 d . . . . .
H42A H 1.0082 0.6439 0.6580 0.053 Uiso 1 1 calc R U . . .
H42B H 0.9993 0.5994 0.7128 0.053 Uiso 1 1 calc R U . . .
H42C H 0.8842 0.6164 0.6419 0.053 Uiso 1 1 calc R U . . .
C43 C 1.0872(8) 0.5491(3) 0.6178(6) 0.041(2) Uani 1 1 d . . . . .
H43A H 1.1102 0.5347 0.5671 0.061 Uiso 1 1 calc R U . . .
H43B H 1.0410 0.5281 0.6462 0.061 Uiso 1 1 calc R U . . .
H43C H 1.1604 0.5582 0.6600 0.061 Uiso 1 1 calc R U . . .
S1 S 0.7623(2) 0.51827(9) 0.61438(16) 0.0450(6) Uani 1 1 d . . . . .
F1 F 0.5541(5) 0.4770(2) 0.5771(4) 0.0658(17) Uani 1 1 d . . . . .
F2 F 0.7036(6) 0.4369(2) 0.6362(5) 0.0679(18) Uani 1 1 d . . . . .
F3 F 0.6280(6) 0.4835(2) 0.7136(4) 0.0654(18) Uani 1 1 d . . . . .
O1 O 0.7006(7) 0.5595(2) 0.6167(6) 0.065(2) Uani 1 1 d . . . . .
O2 O 0.7787(6) 0.5068(2) 0.5280(4) 0.0483(16) Uani 1 1 d . . . . .
O3 O 0.8643(6) 0.5098(3) 0.6848(5) 0.067(2) Uani 1 1 d . . . . .
C44 C 0.6595(9) 0.4771(3) 0.6369(7) 0.047(2) Uani 1 1 d . . . . .
S2 S 0.3138(4) 0.67721(10) -0.00975(17) 0.0716(10) Uani 1 1 d . . . . .
F4 F 0.2926(7) 0.6654(3) -0.1743(5) 0.0846(13) Uani 1 1 d . . . . .
F5 F 0.4783(7) 0.6684(3) -0.0928(5) 0.0846(13) Uani 1 1 d . . . . .
F6 F 0.3577(7) 0.6090(3) -0.0944(5) 0.0846(13) Uani 1 1 d . . . . .
O4 O 0.1771(6) 0.6557(2) -0.0375(5) 0.0579(11) Uani 1 1 d . . . . .
O5 O 0.3053(6) 0.7228(2) -0.0215(5) 0.0579(11) Uani 1 1 d . . . . .
O6 O 0.3717(6) 0.6581(2) 0.0693(5) 0.0579(11) Uani 1 1 d . . . . .
C45 C 0.3514(14) 0.6524(4) -0.1001(7) 0.0716(10) Uani 1 1 d . . . . .
Cl1 Cl 0.3336(3) 0.61749(9) 0.5786(2) 0.0705(9) Uani 1 1 d . . . . .
Cl2 Cl 0.4398(3) 0.56719(10) 0.73360(19) 0.0625(7) Uani 1 1 d . . . . .
C46 C 0.4185(9) 0.5707(3) 0.6193(7) 0.052(3) Uani 1 1 d . U . . .
H46A H 0.4984 0.5722 0.6025 0.063 Uiso 1 1 calc R U . . .
H46B H 0.3763 0.5437 0.5924 0.063 Uiso 1 1 calc R U . . .
Cl3 Cl 0.5974(3) 0.82996(12) -0.0119(2) 0.0807(10) Uani 1 1 d . . . . .
Cl4 Cl 0.7136(3) 0.74885(12) -0.0513(2) 0.0752(9) Uani 1 1 d . . . . .
C47 C 0.5822(13) 0.7759(4) -0.0588(10) 0.089(4) Uani 1 1 d . U . . .
H47A H 0.5287 0.7581 -0.0291 0.107 Uiso 1 1 calc R U . . .
H47B H 0.5421 0.7784 -0.1217 0.107 Uiso 1 1 calc R U . . .
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 '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'
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 C2 147.9(3) . . ?
C1 Ge1 N1 104.6(3) . . ?
C2 Ge1 N1 107.5(3) . . ?
C1 Ge1 P2 83.0(2) . . ?
C2 Ge1 P2 97.2(2) . . ?
N1 Ge1 P2 89.89(17) . . ?
C1 Ge1 P1 97.0(2) . . ?
C2 Ge1 P1 82.5(2) . . ?
N1 Ge1 P1 90.53(17) . . ?
P2 Ge1 P1 179.57(7) . . ?
C3 C1 C11 119.1(6) . . ?
C3 C1 Ge1 123.0(5) . . ?
C11 C1 Ge1 116.6(5) . . ?
C20 P1 C25 108.1(3) . . ?
C20 P1 C28 103.9(3) . . ?
C25 P1 C28 105.3(4) . . ?
C20 P1 Ge1 92.8(2) . . ?
C25 P1 Ge1 127.5(3) . . ?
C28 P1 Ge1 115.8(3) . . ?
C9 P2 C34 108.8(4) . . ?
C9 P2 C31 104.3(3) . . ?
C34 P2 C31 106.4(4) . . ?
C9 P2 Ge1 93.1(3) . . ?
C34 P2 Ge1 126.1(3) . . ?
C31 P2 Ge1 115.0(2) . . ?
C14 C2 C22 118.9(7) . . ?
C14 C2 Ge1 122.8(6) . . ?
C22 C2 Ge1 117.7(5) . . ?
C37 N1 C41 121.6(6) . . ?
C37 N1 Ge1 120.3(5) . . ?
C41 N1 Ge1 118.1(5) . . ?
C39 N2 C42 121.6(7) . . ?
C39 N2 C43 121.8(7) . . ?
C42 N2 C43 116.5(7) . . ?
C1 C3 C4 122.7(7) . . ?
C1 C3 H3 118.7 . . ?
C4 C3 H3 118.7 . . ?
C5 C4 C3 119.3(7) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C4 C5 C10 118.2(7) . . ?
C4 C5 C12 132.3(7) . . ?
C10 C5 C12 109.5(6) . . ?
C7 C6 C10 119.4(7) . . ?
C7 C6 C13 132.0(7) . . ?
C10 C6 C13 108.6(7) . . ?
C6 C7 C8 118.8(7) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 H7 120.6 . . ?
C9 C8 C7 122.9(7) . . ?
C9 C8 H8 118.5 . . ?
C7 C8 H8 118.5 . . ?
C8 C9 C11 119.4(7) . . ?
C8 C9 P2 126.5(6) . . ?
C11 C9 P2 114.0(5) . . ?
C5 C10 C6 112.6(7) . . ?
C5 C10 C11 124.2(7) . . ?
C6 C10 C11 123.2(7) . . ?
C10 C11 C9 116.3(6) . . ?
C10 C11 C1 116.4(6) . . ?
C9 C11 C1 127.3(6) . . ?
C5 C12 C13 104.5(6) . . ?
C5 C12 H12A 110.9 . . ?
C13 C12 H12A 110.9 . . ?
C5 C12 H12B 110.9 . . ?
C13 C12 H12B 110.9 . . ?
H12A C12 H12B 108.9 . . ?
C6 C13 C12 104.6(6) . . ?
C6 C13 H13A 110.8 . . ?
C12 C13 H13A 110.8 . . ?
C6 C13 H13B 110.8 . . ?
C12 C13 H13B 110.8 . . ?
H13A C13 H13B 108.9 . . ?
C2 C14 C15 122.4(7) . . ?
C2 C14 H14 118.8 . . ?
C15 C14 H14 118.8 . . ?
C16 C15 C14 119.3(7) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C15 C16 C21 118.6(7) . . ?
C15 C16 C24 132.8(8) . . ?
C21 C16 C24 108.6(7) . . ?
C18 C17 C21 118.2(7) . . ?
C18 C17 C23 132.7(7) . . ?
C21 C17 C23 109.1(7) . . ?
C17 C18 C19 119.8(7) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C20 C19 C18 121.6(7) . . ?
C20 C19 H19 119.2 . . ?
C18 C19 H19 119.2 . . ?
C19 C20 C22 119.6(7) . . ?
C19 C20 P1 126.0(6) . . ?
C22 C20 P1 114.2(5) . . ?
C22 C21 C16 123.6(7) . . ?
C22 C21 C17 124.0(7) . . ?
C16 C21 C17 112.3(7) . . ?
C21 C22 C20 116.4(7) . . ?
C21 C22 C2 117.1(7) . . ?
C20 C22 C2 126.5(6) . . ?
C17 C23 C24 104.4(7) . . ?
C17 C23 H23A 110.9 . . ?
C24 C23 H23A 110.9 . . ?
C17 C23 H23B 110.9 . . ?
C24 C23 H23B 110.9 . . ?
H23A C23 H23B 108.9 . . ?
C16 C24 C23 105.6(7) . . ?
C16 C24 H24A 110.6 . . ?
C23 C24 H24A 110.6 . . ?
C16 C24 H24B 110.6 . . ?
C23 C24 H24B 110.6 . . ?
H24A C24 H24B 108.8 . . ?
C27 C25 C26 110.8(6) . . ?
C27 C25 P1 110.8(5) . . ?
C26 C25 P1 112.0(5) . . ?
C27 C25 H25 107.7 . . ?
C26 C25 H25 107.7 . . ?
P1 C25 H25 107.7 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C30 C28 C29 111.4(7) . . ?
C30 C28 P1 110.6(6) . . ?
C29 C28 P1 113.7(5) . . ?
C30 C28 H28 106.9 . . ?
C29 C28 H28 106.9 . . ?
P1 C28 H28 106.9 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 C33 111.5(7) . . ?
C32 C31 P2 109.2(5) . . ?
C33 C31 P2 112.6(5) . . ?
C32 C31 H31 107.8 . . ?
C33 C31 H31 107.8 . . ?
P2 C31 H31 107.8 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C36 C34 C35 112.5(7) . . ?
C36 C34 P2 112.7(5) . . ?
C35 C34 P2 109.0(5) . . ?
C36 C34 H34 107.5 . . ?
C35 C34 H34 107.5 . . ?
P2 C34 H34 107.5 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N1 C37 C38 121.8(7) . . ?
N1 C37 H37 119.1 . . ?
C38 C37 H37 119.1 . . ?
C37 C38 C39 119.1(7) . . ?
C37 C38 H38 120.4 . . ?
C39 C38 H38 120.4 . . ?
N2 C39 C40 121.5(7) . . ?
N2 C39 C38 121.8(7) . . ?
C40 C39 C38 116.7(7) . . ?
C41 C40 C39 119.6(7) . . ?
C41 C40 H40 120.2 . . ?
C39 C40 H40 120.2 . . ?
N1 C41 C40 121.1(7) . . ?
N1 C41 H41 119.4 . . ?
C40 C41 H41 119.4 . . ?
N2 C42 H42A 109.5 . . ?
N2 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
N2 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N2 C43 H43A 109.5 . . ?
N2 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
N2 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O1 S1 O2 113.1(5) . . ?
O1 S1 O3 116.9(5) . . ?
O2 S1 O3 115.5(5) . . ?
O1 S1 C44 105.0(5) . . ?
O2 S1 C44 103.4(5) . . ?
O3 S1 C44 100.3(5) . . ?
F2 C44 F3 108.4(8) . . ?
F2 C44 F1 106.0(9) . . ?
F3 C44 F1 104.7(8) . . ?
F2 C44 S1 112.1(7) . . ?
F3 C44 S1 112.5(7) . . ?
F1 C44 S1 112.6(7) . . ?
O5 S2 O6 122.2(5) . . ?
O5 S2 O4 108.6(4) . . ?
O6 S2 O4 108.2(4) . . ?
O5 S2 C45 110.1(5) . . ?
O6 S2 C45 113.1(5) . . ?
O4 S2 C45 89.6(6) . . ?
F4 C45 F6 112.2(11) . . ?
F4 C45 F5 106.4(10) . . ?
F6 C45 F5 106.2(9) . . ?
F4 C45 S2 116.0(8) . . ?
F6 C45 S2 113.4(8) . . ?
F5 C45 S2 101.2(9) . . ?
Cl1 C46 Cl2 111.5(6) . . ?
Cl1 C46 H46A 109.3 . . ?
Cl2 C46 H46A 109.3 . . ?
Cl1 C46 H46B 109.3 . . ?
Cl2 C46 H46B 109.3 . . ?
H46A C46 H46B 108.0 . . ?
Cl4 C47 Cl3 114.1(8) . . ?
Cl4 C47 H47A 108.7 . . ?
Cl3 C47 H47A 108.7 . . ?
Cl4 C47 H47B 108.7 . . ?
Cl3 C47 H47B 108.7 . . ?
H47A C47 H47B 107.6 . . ?
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 1.951(7) . ?
Ge1 C2 1.954(7) . ?
Ge1 N1 1.964(6) . ?
Ge1 P2 2.596(3) . ?
Ge1 P1 2.610(3) . ?
C1 C3 1.364(10) . ?
C1 C11 1.420(10) . ?
P1 C20 1.788(7) . ?
P1 C25 1.823(7) . ?
P1 C28 1.837(7) . ?
P2 C9 1.789(7) . ?
P2 C34 1.837(8) . ?
P2 C31 1.849(7) . ?
C2 C14 1.381(10) . ?
C2 C22 1.421(10) . ?
N1 C37 1.300(10) . ?
N1 C41 1.333(9) . ?
N2 C39 1.331(10) . ?
N2 C42 1.447(10) . ?
N2 C43 1.469(11) . ?
C3 C4 1.406(10) . ?
C3 H3 0.9500 . ?
C4 C5 1.371(11) . ?
C4 H4 0.9500 . ?
C5 C10 1.378(10) . ?
C5 C12 1.504(10) . ?
C6 C7 1.362(11) . ?
C6 C10 1.398(10) . ?
C6 C13 1.509(11) . ?
C7 C8 1.392(11) . ?
C7 H7 0.9500 . ?
C8 C9 1.383(10) . ?
C8 H8 0.9500 . ?
C9 C11 1.416(10) . ?
C10 C11 1.404(10) . ?
C12 C13 1.550(11) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.406(11) . ?
C14 H14 0.9500 . ?
C15 C16 1.363(12) . ?
C15 H15 0.9500 . ?
C16 C21 1.400(11) . ?
C16 C24 1.502(11) . ?
C17 C18 1.354(12) . ?
C17 C21 1.401(11) . ?
C17 C23 1.507(11) . ?
C18 C19 1.408(10) . ?
C18 H18 0.9500 . ?
C19 C20 1.383(10) . ?
C19 H19 0.9500 . ?
C20 C22 1.415(10) . ?
C21 C22 1.390(10) . ?
C23 C24 1.548(13) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C27 1.519(10) . ?
C25 C26 1.520(11) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C30 1.511(12) . ?
C28 C29 1.526(10) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.509(11) . ?
C31 C33 1.526(10) . ?
C31 H31 1.0000 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C36 1.498(11) . ?
C34 C35 1.515(11) . ?
C34 H34 1.0000 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.364(11) . ?
C37 H37 0.9500 . ?
C38 C39 1.422(11) . ?
C38 H38 0.9500 . ?
C39 C40 1.404(11) . ?
C40 C41 1.362(10) . ?
C40 H40 0.9500 . ?
C41 H41 0.9500 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
S1 O1 1.426(7) . ?
S1 O2 1.434(7) . ?
S1 O3 1.435(7) . ?
S1 C44 1.781(11) . ?
F1 C44 1.347(12) . ?
F2 C44 1.308(11) . ?
F3 C44 1.327(11) . ?
S2 O5 1.384(8) . ?
S2 O6 1.388(7) . ?
S2 O4 1.644(8) . ?
S2 C45 1.718(11) . ?
F4 C45 1.265(12) . ?
F5 C45 1.492(17) . ?
F6 C45 1.311(13) . ?
Cl1 C46 1.743(10) . ?
Cl2 C46 1.744(11) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
Cl3 C47 1.774(15) . ?
Cl4 C47 1.673(15) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11 C1 C3 C4 -1.0(11) . . . . ?
Ge1 C1 C3 C4 165.4(6) . . . . ?
C1 C3 C4 C5 -3.1(11) . . . . ?
C3 C4 C5 C10 3.3(10) . . . . ?
C3 C4 C5 C12 -176.3(7) . . . . ?
C10 C6 C7 C8 0.0(11) . . . . ?
C13 C6 C7 C8 177.9(8) . . . . ?
C6 C7 C8 C9 -0.2(12) . . . . ?
C7 C8 C9 C11 -0.5(11) . . . . ?
C7 C8 C9 P2 175.3(6) . . . . ?
C34 P2 C9 C8 35.8(8) . . . . ?
C31 P2 C9 C8 -77.5(7) . . . . ?
Ge1 P2 C9 C8 165.7(7) . . . . ?
C34 P2 C9 C11 -148.2(5) . . . . ?
C31 P2 C9 C11 98.5(6) . . . . ?
Ge1 P2 C9 C11 -18.3(5) . . . . ?
C4 C5 C10 C6 -180.0(7) . . . . ?
C12 C5 C10 C6 -0.3(9) . . . . ?
C4 C5 C10 C11 0.4(11) . . . . ?
C12 C5 C10 C11 -179.9(7) . . . . ?
C7 C6 C10 C5 -178.7(7) . . . . ?
C13 C6 C10 C5 2.9(9) . . . . ?
C7 C6 C10 C11 0.9(11) . . . . ?
C13 C6 C10 C11 -177.5(7) . . . . ?
C5 C10 C11 C9 178.0(7) . . . . ?
C6 C10 C11 C9 -1.5(10) . . . . ?
C5 C10 C11 C1 -4.3(10) . . . . ?
C6 C10 C11 C1 176.1(7) . . . . ?
C8 C9 C11 C10 1.3(10) . . . . ?
P2 C9 C11 C10 -175.0(5) . . . . ?
C8 C9 C11 C1 -176.1(7) . . . . ?
P2 C9 C11 C1 7.6(10) . . . . ?
C3 C1 C11 C10 4.5(10) . . . . ?
Ge1 C1 C11 C10 -162.8(5) . . . . ?
C3 C1 C11 C9 -178.2(7) . . . . ?
Ge1 C1 C11 C9 14.6(10) . . . . ?
C4 C5 C12 C13 177.3(8) . . . . ?
C10 C5 C12 C13 -2.3(8) . . . . ?
C7 C6 C13 C12 177.7(8) . . . . ?
C10 C6 C13 C12 -4.2(8) . . . . ?
C5 C12 C13 C6 3.8(8) . . . . ?
C22 C2 C14 C15 0.2(12) . . . . ?
Ge1 C2 C14 C15 170.7(6) . . . . ?
C2 C14 C15 C16 -2.8(13) . . . . ?
C14 C15 C16 C21 1.9(14) . . . . ?
C14 C15 C16 C24 -175.7(10) . . . . ?
C21 C17 C18 C19 4.4(11) . . . . ?
C23 C17 C18 C19 -176.3(8) . . . . ?
C17 C18 C19 C20 -2.2(11) . . . . ?
C18 C19 C20 C22 -3.3(11) . . . . ?
C18 C19 C20 P1 171.3(6) . . . . ?
C25 P1 C20 C19 32.8(7) . . . . ?
C28 P1 C20 C19 -78.7(7) . . . . ?
Ge1 P1 C20 C19 163.9(6) . . . . ?
C25 P1 C20 C22 -152.3(5) . . . . ?
C28 P1 C20 C22 96.2(6) . . . . ?
Ge1 P1 C20 C22 -21.2(5) . . . . ?
C15 C16 C21 C22 1.5(13) . . . . ?
C24 C16 C21 C22 179.7(8) . . . . ?
C15 C16 C21 C17 -176.6(8) . . . . ?
C24 C16 C21 C17 1.5(11) . . . . ?
C18 C17 C21 C22 -1.3(12) . . . . ?
C23 C17 C21 C22 179.2(7) . . . . ?
C18 C17 C21 C16 176.8(8) . . . . ?
C23 C17 C21 C16 -2.7(10) . . . . ?
C16 C21 C22 C20 178.1(7) . . . . ?
C17 C21 C22 C20 -4.0(11) . . . . ?
C16 C21 C22 C2 -4.0(11) . . . . ?
C17 C21 C22 C2 173.9(7) . . . . ?
C19 C20 C22 C21 6.1(10) . . . . ?
P1 C20 C22 C21 -169.1(5) . . . . ?
C19 C20 C22 C2 -171.6(7) . . . . ?
P1 C20 C22 C2 13.2(10) . . . . ?
C14 C2 C22 C21 3.0(10) . . . . ?
Ge1 C2 C22 C21 -167.9(5) . . . . ?
C14 C2 C22 C20 -179.3(7) . . . . ?
Ge1 C2 C22 C20 9.8(10) . . . . ?
C18 C17 C23 C24 -176.8(9) . . . . ?
C21 C17 C23 C24 2.6(10) . . . . ?
C15 C16 C24 C23 178.0(10) . . . . ?
C21 C16 C24 C23 0.2(11) . . . . ?
C17 C23 C24 C16 -1.6(10) . . . . ?
C20 P1 C25 C27 -171.4(6) . . . . ?
C28 P1 C25 C27 -60.9(6) . . . . ?
Ge1 P1 C25 C27 80.2(6) . . . . ?
C20 P1 C25 C26 64.3(6) . . . . ?
C28 P1 C25 C26 174.8(5) . . . . ?
Ge1 P1 C25 C26 -44.1(6) . . . . ?
C20 P1 C28 C30 -66.1(6) . . . . ?
C25 P1 C28 C30 -179.7(6) . . . . ?
Ge1 P1 C28 C30 33.9(6) . . . . ?
C20 P1 C28 C29 60.0(7) . . . . ?
C25 P1 C28 C29 -53.5(7) . . . . ?
Ge1 P1 C28 C29 160.1(5) . . . . ?
C9 P2 C31 C32 -70.0(6) . . . . ?
C34 P2 C31 C32 175.2(5) . . . . ?
Ge1 P2 C31 C32 30.4(6) . . . . ?
C9 P2 C31 C33 54.5(7) . . . . ?
C34 P2 C31 C33 -60.4(7) . . . . ?
Ge1 P2 C31 C33 154.9(5) . . . . ?
C9 P2 C34 C36 54.1(7) . . . . ?
C31 P2 C34 C36 165.9(6) . . . . ?
Ge1 P2 C34 C36 -54.5(7) . . . . ?
C9 P2 C34 C35 179.7(6) . . . . ?
C31 P2 C34 C35 -68.5(7) . . . . ?
Ge1 P2 C34 C35 71.1(7) . . . . ?
C41 N1 C37 C38 -0.4(11) . . . . ?
Ge1 N1 C37 C38 179.8(6) . . . . ?
N1 C37 C38 C39 0.4(12) . . . . ?
C42 N2 C39 C40 176.6(8) . . . . ?
C43 N2 C39 C40 -1.0(12) . . . . ?
C42 N2 C39 C38 -2.7(12) . . . . ?
C43 N2 C39 C38 179.7(8) . . . . ?
C37 C38 C39 N2 179.3(8) . . . . ?
C37 C38 C39 C40 -0.1(11) . . . . ?
N2 C39 C40 C41 -179.5(7) . . . . ?
C38 C39 C40 C41 -0.1(11) . . . . ?
C37 N1 C41 C40 0.2(11) . . . . ?
Ge1 N1 C41 C40 179.9(6) . . . . ?
C39 C40 C41 N1 0.1(12) . . . . ?
O1 S1 C44 F2 179.4(7) . . . . ?
O2 S1 C44 F2 60.7(8) . . . . ?
O3 S1 C44 F2 -58.9(8) . . . . ?
O1 S1 C44 F3 -58.1(8) . . . . ?
O2 S1 C44 F3 -176.8(7) . . . . ?
O3 S1 C44 F3 63.6(8) . . . . ?
O1 S1 C44 F1 60.0(8) . . . . ?
O2 S1 C44 F1 -58.8(8) . . . . ?
O3 S1 C44 F1 -178.3(7) . . . . ?
O5 S2 C45 F4 -46.2(14) . . . . ?
O6 S2 C45 F4 173.2(10) . . . . ?
O4 S2 C45 F4 63.5(12) . . . . ?
O5 S2 C45 F6 -178.2(9) . . . . ?
O6 S2 C45 F6 41.2(13) . . . . ?
O4 S2 C45 F6 -68.5(11) . . . . ?
O5 S2 C45 F5 68.5(7) . . . . ?
O6 S2 C45 F5 -72.1(8) . . . . ?
O4 S2 C45 F5 178.2(6) . . . . ?
