 
data_TT_0m_a
 
_audit_creation_method            'SHELXL-2017/1'
_shelx_SHELXL_version_number      '2017/1'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C55 H50 Cl12 Ge N4 O4' 
_chemical_formula_weight          1328.98

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'
 'Ge'  'Ge'   0.1547   1.8001
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       triclinic
_space_group_IT_number            2
_space_group_name_H-M_alt         'P -1'
_space_group_name_Hall            '-P 1'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    9.0522(6)
_cell_length_b                    12.8275(9)
_cell_length_c                    25.9222(19)
_cell_angle_alpha                 85.175(3)
_cell_angle_beta                  82.476(3)
_cell_angle_gamma                 78.104(3)
_cell_volume                      2914.9(4)
_cell_formula_units_Z             2
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used     9961
_cell_measurement_theta_min       2.34
_cell_measurement_theta_max       28.57
 
_exptl_crystal_description        'plate'
_exptl_crystal_colour             'colourless'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.514          
_exptl_crystal_F_000              1352
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.27
_exptl_crystal_size_mid           0.12
_exptl_crystal_size_min           0.03
_exptl_absorpt_coefficient_mu     1.124
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.6610
_exptl_absorpt_correction_T_max   0.7457
_exptl_absorpt_process_details    'Bruker SADABS'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             101054
_diffrn_reflns_av_unetI/netI      0.0363
_diffrn_reflns_av_R_equivalents   0.0521
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -34
_diffrn_reflns_limit_l_max        34
_diffrn_reflns_theta_min          0.794
_diffrn_reflns_theta_max          28.665
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.987
_diffrn_measured_fraction_theta_full  0.999
_diffrn_reflns_Laue_measured_fraction_max    0.987
_diffrn_reflns_Laue_measured_fraction_full   0.999
_diffrn_reflns_point_group_measured_fraction_max   0.987
_diffrn_reflns_point_group_measured_fraction_full  0.999
_reflns_number_total              14820
_reflns_number_gt                 12581
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0344P)²+7.0305P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          14820
_refine_ls_number_parameters      693
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0658
_refine_ls_R_factor_gt            0.0530
_refine_ls_wR_factor_ref          0.1174
_refine_ls_wR_factor_gt           0.1112
_refine_ls_goodness_of_fit_ref    1.067
_refine_ls_restrained_S_all       1.067
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Ge1 Ge 0.26949(3) 0.26994(2) 0.75173(2) 0.01418(7) Uani 1 1 d . . . . .
Cl1 Cl 0.12918(9) 0.59940(6) 0.84070(3) 0.03092(16) Uani 1 1 d . . . . .
Cl2 Cl 0.27594(10) 0.57136(7) 0.94581(3) 0.0397(2) Uani 1 1 d . . . . .
Cl3 Cl 0.49610(9) 0.35648(8) 0.97370(3) 0.0386(2) Uani 1 1 d . . . . .
Cl4 Cl 0.56170(8) 0.16883(6) 0.89627(3) 0.02752(15) Uani 1 1 d . . . . .
Cl5 Cl 0.62133(9) 0.34471(6) 0.60488(3) 0.02949(16) Uani 1 1 d . . . . .
Cl6 Cl 0.70541(10) 0.15098(7) 0.53099(3) 0.03533(18) Uani 1 1 d . . . . .
Cl7 Cl 0.56793(11) -0.05417(7) 0.56295(3) 0.0381(2) Uani 1 1 d . . . . .
Cl8 Cl 0.34458(8) -0.06249(5) 0.66709(3) 0.02725(15) Uani 1 1 d . . . . .
Cl9 Cl 0.8002(2) 0.42473(9) 0.86382(4) 0.0803(5) Uani 1 1 d . . . . .
Cl10 Cl 0.65064(16) 0.64157(9) 0.88359(5) 0.0744(4) Uani 1 1 d . . . . .
Cl11 Cl 1.0313(2) -0.09648(17) 0.36833(6) 0.1063(6) Uani 1 1 d . . . . .
Cl12 Cl 0.9923(2) 0.10412(15) 0.42197(8) 0.1050(6) Uani 1 1 d . . . . .
N1 N 0.1148(2) 0.15452(17) 0.84576(8) 0.0157(4) Uani 1 1 d . . . . .
N2 N -0.0379(2) 0.21149(16) 0.78126(8) 0.0144(4) Uani 1 1 d . . . . .
N3 N 0.1243(2) 0.39307(17) 0.66210(9) 0.0170(4) Uani 1 1 d . . . . .
N4 N -0.0524(2) 0.34798(17) 0.72661(8) 0.0151(4) Uani 1 1 d . . . . .
O1 O 0.2198(2) 0.40442(14) 0.77926(8) 0.0196(4) Uani 1 1 d . . . . .
O2 O 0.3894(2) 0.22403(14) 0.80388(7) 0.0166(4) Uani 1 1 d . . . . .
O3 O 0.4080(2) 0.30520(14) 0.69868(7) 0.0175(4) Uani 1 1 d . . . . .
O4 O 0.2966(2) 0.13559(15) 0.72487(8) 0.0191(4) Uani 1 1 d . . . . .
C1 C 0.2794(3) 0.3993(2) 0.82423(10) 0.0171(5) Uani 1 1 d . . . . .
C2 C 0.2501(3) 0.4822(2) 0.85760(11) 0.0220(6) Uani 1 1 d . . . . .
C3 C 0.3172(3) 0.4685(2) 0.90392(12) 0.0253(6) Uani 1 1 d . . . . .
C4 C 0.4144(3) 0.3732(3) 0.91633(11) 0.0259(6) Uani 1 1 d . . . . .
C5 C 0.4425(3) 0.2889(2) 0.88281(11) 0.0202(5) Uani 1 1 d . . . . .
C6 C 0.3731(3) 0.3017(2) 0.83765(10) 0.0162(5) Uani 1 1 d . . . . .
C7 C 0.1917(3) 0.0844(2) 0.88432(10) 0.0165(5) Uani 1 1 d . . . . .
C8 C 0.1707(3) 0.1231(2) 0.93478(11) 0.0209(5) Uani 1 1 d . . . . .
C9 C 0.2461(4) 0.0602(3) 0.97366(12) 0.0292(7) Uani 1 1 d . . . . .
H9 H 0.231062 0.084018 1.008037 0.035 Uiso 1 1 calc R U . . .
C10 C 0.3425(4) -0.0363(3) 0.96298(12) 0.0312(7) Uani 1 1 d . . . . .
H10 H 0.392420 -0.078604 0.989894 0.037 Uiso 1 1 calc R U . . .
C11 C 0.3656(3) -0.0707(2) 0.91292(12) 0.0258(6) Uani 1 1 d . . . . .
H11 H 0.433385 -0.136357 0.905829 0.031 Uiso 1 1 calc R U . . .
C12 C 0.2922(3) -0.0119(2) 0.87226(11) 0.0192(5) Uani 1 1 d . . . . .
C13 C 0.0635(3) 0.2289(2) 0.94655(12) 0.0254(6) Uani 1 1 d . . . . .
H13 H 0.069857 0.277573 0.914460 0.030 Uiso 1 1 calc R U . . .
C14 C 0.1029(4) 0.2849(3) 0.99120(14) 0.0369(8) Uani 1 1 d . . . . .
H14A H 0.074572 0.247745 1.024482 0.055 Uiso 1 1 calc R U . . .
H14B H 0.047110 0.358953 0.990779 0.055 Uiso 1 1 calc R U . . .
H14C H 0.212405 0.283772 0.986949 0.055 Uiso 1 1 calc R U . . .
C15 C -0.1002(4) 0.2128(3) 0.95783(15) 0.0368(8) Uani 1 1 d . . . . .
H15A H -0.128550 0.183988 0.927538 0.055 Uiso 1 1 calc R U . . .
H15B H -0.167950 0.281451 0.964965 0.055 Uiso 1 1 calc R U . . .
H15C H -0.109186 0.162745 0.988237 0.055 Uiso 1 1 calc R U . . .
C16 C 0.3330(3) -0.0518(2) 0.81771(11) 0.0202(5) Uani 1 1 d . . . . .
H16 H 0.267417 -0.003073 0.793983 0.024 Uiso 1 1 calc R U . . .
C17 C 0.3049(4) -0.1655(2) 0.81530(14) 0.0306(7) Uani 1 1 d . . . . .
H17A H 0.370503 -0.215051 0.837498 0.046 Uiso 1 1 calc R U . . .
H17B H 0.327947 -0.186922 0.779260 0.046 Uiso 1 1 calc R U . . .
H17C H 0.198174 -0.166951 0.827614 0.046 Uiso 1 1 calc R U . . .
C18 C 0.4991(3) -0.0484(2) 0.79820(13) 0.0268(6) Uani 1 1 d . . . . .
H18A H 0.515690 0.024463 0.799226 0.040 Uiso 1 1 calc R U . . .
H18B H 0.522397 -0.070723 0.762309 0.040 Uiso 1 1 calc R U . . .
H18C H 0.565565 -0.096812 0.820569 0.040 Uiso 1 1 calc R U . . .
C19 C 0.0207(3) 0.1291(2) 0.81994(10) 0.0153(5) Uani 1 1 d . . . . .
C20 C -0.0385(3) 0.0295(2) 0.82006(10) 0.0162(5) Uani 1 1 d . . . . .
C21 C -0.0773(3) -0.0268(2) 0.86663(11) 0.0215(6) Uani 1 1 d . . . . .
H21 H -0.071708 0.000299 0.899176 0.026 Uiso 1 1 calc R U . . .
C22 C -0.1242(3) -0.1230(2) 0.86484(13) 0.0278(6) Uani 1 1 d . . . . .
H22 H -0.153029 -0.160978 0.896353 0.033 Uiso 1 1 calc R U . . .
C23 C -0.1291(3) -0.1637(2) 0.81757(13) 0.0276(7) Uani 1 1 d . . . . .
H23 H -0.157227 -0.230864 0.816781 0.033 Uiso 1 1 calc R U . . .
C24 C -0.0933(3) -0.1072(2) 0.77135(13) 0.0263(6) Uani 1 1 d . . . . .
H24 H -0.099404 -0.134609 0.738932 0.032 Uiso 1 1 calc R U . . .
C25 C -0.0483(3) -0.0100(2) 0.77254(11) 0.0205(5) Uani 1 1 d . . . . .
H25 H -0.024213 0.029226 0.740902 0.025 Uiso 1 1 calc R U . . .
C26 C 0.0451(3) 0.27745(19) 0.75375(9) 0.0135(5) Uani 1 1 d . . . . .
C27 C -0.1888(3) 0.2396(2) 0.77074(11) 0.0193(5) Uani 1 1 d . . . . .
H27 H -0.269450 0.204828 0.784817 0.023 Uiso 1 1 calc R U . . .
C28 C -0.1980(3) 0.3253(2) 0.73687(11) 0.0191(5) Uani 1 1 d . . . . .
H28 H -0.286614 0.363184 0.722637 0.023 Uiso 1 1 calc R U . . .
C29 C -0.0041(3) 0.4262(2) 0.68716(10) 0.0149(5) Uani 1 1 d . . . . .
C30 C -0.1119(3) 0.5299(2) 0.68466(10) 0.0154(5) Uani 1 1 d . . . . .
C31 C -0.1858(3) 0.5749(2) 0.73050(11) 0.0193(5) Uani 1 1 d . . . . .
H31 H -0.173301 0.536207 0.763049 0.023 Uiso 1 1 calc R U . . .
C32 C -0.2778(3) 0.6760(2) 0.72895(12) 0.0236(6) Uani 1 1 d . . . . .
H32 H -0.327640 0.706314 0.760377 0.028 Uiso 1 1 calc R U . . .
C33 C -0.2968(3) 0.7326(2) 0.68165(13) 0.0277(6) Uani 1 1 d . . . . .
H33 H -0.358904 0.801983 0.680653 0.033 Uiso 1 1 calc R U . . .
C34 C -0.2254(4) 0.6882(2) 0.63572(12) 0.0279(6) Uani 1 1 d . . . . .
H34 H -0.239916 0.727092 0.603326 0.033 Uiso 1 1 calc R U . . .
C35 C -0.1328(3) 0.5874(2) 0.63666(11) 0.0219(6) Uani 1 1 d . . . . .
H35 H -0.083803 0.557454 0.605066 0.026 Uiso 1 1 calc R U . . .
C36 C 0.1950(3) 0.4574(2) 0.62235(10) 0.0170(5) Uani 1 1 d . . . . .
C37 C 0.2471(3) 0.5482(2) 0.63323(11) 0.0195(5) Uani 1 1 d . . . . .
C38 C 0.3165(3) 0.6038(2) 0.59125(12) 0.0276(6) Uani 1 1 d . . . . .
H38 H 0.352440 0.665536 0.597565 0.033 Uiso 1 1 calc R U . . .
C39 C 0.3341(4) 0.5715(3) 0.54108(12) 0.0320(7) Uani 1 1 d . . . . .
H39 H 0.378593 0.611914 0.513117 0.038 Uiso 1 1 calc R U . . .
C40 C 0.2866(4) 0.4800(3) 0.53181(12) 0.0317(7) Uani 1 1 d . . . . .
H40 H 0.300884 0.457324 0.497241 0.038 Uiso 1 1 calc R U . . .
C41 C 0.2182(3) 0.4200(2) 0.57173(11) 0.0234(6) Uani 1 1 d . . . . .
C42 C 0.2377(3) 0.5859(2) 0.68777(11) 0.0208(5) Uani 1 1 d . . . . .
H42 H 0.178987 0.540586 0.712233 0.025 Uiso 1 1 calc R U . . .
C43 C 0.3974(4) 0.5711(3) 0.70465(13) 0.0305(7) Uani 1 1 d . . . . .
H43A H 0.448266 0.496081 0.702540 0.046 Uiso 1 1 calc R U . . .
H43B H 0.389383 0.591772 0.740612 0.046 Uiso 1 1 calc R U . . .
H43C H 0.456548 0.615945 0.681588 0.046 Uiso 1 1 calc R U . . .
C44 C 0.1544(4) 0.7027(2) 0.69170(14) 0.0323(7) Uani 1 1 d . . . . .
H44A H 0.212006 0.749071 0.668971 0.048 Uiso 1 1 calc R U . . .
H44B H 0.145391 0.722698 0.727813 0.048 Uiso 1 1 calc R U . . .
H44C H 0.052780 0.710908 0.680809 0.048 Uiso 1 1 calc R U . . .
C45 C 0.1647(4) 0.3203(3) 0.56080(14) 0.0344(7) Uani 1 1 d . . . . .
H45 H 0.164784 0.273506 0.593672 0.041 Uiso 1 1 calc R U . . .
C46 C 0.2672(5) 0.2561(3) 0.51849(16) 0.0490(10) Uani 1 1 d . . . . .
H46A H 0.258858 0.296061 0.484720 0.074 Uiso 1 1 calc R U . . .
H46B H 0.236045 0.187674 0.517217 0.074 Uiso 1 1 calc R U . . .
H46C H 0.372748 0.243213 0.526249 0.074 Uiso 1 1 calc R U . . .
C47 C 0.0028(4) 0.3478(4) 0.5472(3) 0.0744(18) Uani 1 1 d . . . . .
H47A H -0.063877 0.384326 0.575829 0.112 Uiso 1 1 calc R U . . .
H47B H -0.030818 0.282195 0.541529 0.112 Uiso 1 1 calc R U . . .
H47C H -0.001542 0.394720 0.515312 0.112 Uiso 1 1 calc R U . . .
C48 C 0.3912(3) 0.1329(2) 0.68036(10) 0.0173(5) Uani 1 1 d . . . . .
C49 C 0.4523(3) 0.2246(2) 0.66604(10) 0.0166(5) Uani 1 1 d . . . . .
C50 C 0.5497(3) 0.2297(2) 0.62078(11) 0.0213(5) Uani 1 1 d . . . . .
C51 C 0.5871(3) 0.1428(2) 0.58861(11) 0.0242(6) Uani 1 1 d . . . . .
C52 C 0.5263(3) 0.0522(2) 0.60263(11) 0.0238(6) Uani 1 1 d . . . . .
C53 C 0.4272(3) 0.0472(2) 0.64868(11) 0.0200(5) Uani 1 1 d . . . . .
C54 C 0.7662(5) 0.5266(3) 0.90706(15) 0.0498(10) Uani 1 1 d . . . . .
H54A H 0.717116 0.501717 0.940933 0.060 Uiso 1 1 calc R U . . .
H54B H 0.864361 0.543458 0.913032 0.060 Uiso 1 1 calc R U . . .
C55 C 0.9402(6) -0.0184(5) 0.42192(19) 0.0729(16) Uani 1 1 d . . . . .
H55A H 0.828803 -0.006335 0.421352 0.088 Uiso 1 1 calc R U . . .
H55B H 0.964027 -0.059777 0.454805 0.088 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 O2 1.8273(18) . ?
Ge1 O3 1.8289(18) . ?
Ge1 O1 1.8684(18) . ?
Ge1 O4 1.8703(18) . ?
Ge1 C26 2.007(2) . ?
Cl1 C2 1.728(3) . ?
Cl2 C3 1.730(3) . ?
Cl3 C4 1.724(3) . ?
Cl4 C5 1.727(3) . ?
Cl5 C50 1.729(3) . ?
Cl6 C51 1.729(3) . ?
Cl7 C52 1.728(3) . ?
Cl8 C53 1.731(3) . ?
Cl9 C54 1.746(4) . ?
Cl10 C54 1.737(4) . ?
Cl11 C55 1.791(6) . ?
Cl12 C55 1.732(6) . ?
N1 C19 1.258(3) . ?
N1 C7 1.437(3) . ?
N2 C26 1.345(3) . ?
N2 C27 1.395(3) . ?
N2 C19 1.461(3) . ?
N3 C29 1.265(3) . ?
N3 C36 1.433(3) . ?
N4 C26 1.349(3) . ?
N4 C28 1.394(3) . ?
N4 C29 1.462(3) . ?
O1 C1 1.338(3) . ?
O2 C6 1.354(3) . ?
O3 C49 1.354(3) . ?
O4 C48 1.342(3) . ?
C1 C2 1.388(4) . ?
C1 C6 1.405(4) . ?
C2 C3 1.398(4) . ?
C3 C4 1.391(5) . ?
C4 C5 1.405(4) . ?
C5 C6 1.382(4) . ?
C7 C12 1.407(4) . ?
C7 C8 1.414(4) . ?
C8 C9 1.396(4) . ?
C8 C13 1.525(4) . ?
C9 C10 1.386(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.382(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.401(4) . ?
C11 H11 0.9500 . ?
C12 C16 1.518(4) . ?
C13 C15 1.524(4) . ?
C13 C14 1.529(4) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C18 1.530(4) . ?
C16 C17 1.539(4) . ?
C16 H16 1.0000 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.484(3) . ?
C20 C25 1.391(4) . ?
C20 C21 1.396(4) . ?
C21 C22 1.392(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.381(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.384(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.393(4) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C27 C28 1.344(4) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C30 1.481(4) . ?
C30 C31 1.393(4) . ?
C30 C35 1.406(4) . ?
C31 C32 1.390(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.383(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.386(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.389(4) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.407(4) . ?
C36 C41 1.410(4) . ?
C37 C38 1.400(4) . ?
C37 C42 1.518(4) . ?
C38 C39 1.377(5) . ?
C38 H38 0.9500 . ?
C39 C40 1.379(5) . ?
C39 H39 0.9500 . ?
C40 C41 1.393(4) . ?
C40 H40 0.9500 . ?
C41 C45 1.518(4) . ?
C42 C43 1.535(4) . ?
C42 C44 1.537(4) . ?
C42 H42 1.0000 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C47 1.516(5) . ?
C45 C46 1.521(5) . ?
C45 H45 1.0000 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 C53 1.387(4) . ?
C48 C49 1.402(4) . ?
C49 C50 1.378(4) . ?
C50 C51 1.407(4) . ?
C51 C52 1.388(4) . ?
C52 C53 1.401(4) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O2 Ge1 O3 101.56(8) . . ?
O2 Ge1 O1 88.58(8) . . ?
O3 Ge1 O1 95.63(8) . . ?
O2 Ge1 O4 94.91(8) . . ?
O3 Ge1 O4 88.70(8) . . ?
O1 Ge1 O4 173.80(8) . . ?
O2 Ge1 C26 128.14(9) . . ?
O3 Ge1 C26 130.30(9) . . ?
O1 Ge1 C26 86.85(9) . . ?
O4 Ge1 C26 86.96(9) . . ?
C19 N1 C7 123.9(2) . . ?
C26 N2 C27 110.3(2) . . ?
C26 N2 C19 124.0(2) . . ?
C27 N2 C19 125.6(2) . . ?
C29 N3 C36 122.9(2) . . ?
C26 N4 C28 110.2(2) . . ?
C26 N4 C29 123.3(2) . . ?
C28 N4 C29 126.1(2) . . ?
C1 O1 Ge1 109.19(16) . . ?
C6 O2 Ge1 109.99(16) . . ?
C49 O3 Ge1 109.94(16) . . ?
C48 O4 Ge1 109.07(16) . . ?
O1 C1 C2 124.0(2) . . ?
O1 C1 C6 116.0(2) . . ?
C2 C1 C6 120.0(2) . . ?
C1 C2 C3 119.5(3) . . ?
C1 C2 Cl1 118.6(2) . . ?
C3 C2 Cl1 121.9(2) . . ?
C4 C3 C2 120.5(3) . . ?
C4 C3 Cl2 120.6(2) . . ?
C2 C3 Cl2 118.9(2) . . ?
C3 C4 C5 119.9(3) . . ?
C3 C4 Cl3 120.3(2) . . ?
C5 C4 Cl3 119.7(2) . . ?
C6 C5 C4 119.5(3) . . ?
C6 C5 Cl4 118.5(2) . . ?
C4 C5 Cl4 122.0(2) . . ?
O2 C6 C5 123.7(2) . . ?
O2 C6 C1 115.8(2) . . ?
C5 C6 C1 120.5(2) . . ?
C12 C7 C8 121.5(2) . . ?
C12 C7 N1 122.8(2) . . ?
C8 C7 N1 115.4(2) . . ?
C9 C8 C7 118.3(3) . . ?
C9 C8 C13 121.2(3) . . ?
C7 C8 C13 120.5(2) . . ?
C10 C9 C8 121.1(3) . . ?
C10 C9 H9 119.4 . . ?
C8 C9 H9 119.4 . . ?
C11 C10 C9 119.6(3) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C10 C11 C12 122.1(3) . . ?
C10 C11 H11 118.9 . . ?
C12 C11 H11 118.9 . . ?
C11 C12 C7 117.3(3) . . ?
C11 C12 C16 118.4(2) . . ?
C7 C12 C16 124.1(2) . . ?
C15 C13 C8 110.3(3) . . ?
C15 C13 C14 109.7(3) . . ?
C8 C13 C14 114.2(3) . . ?
C15 C13 H13 107.5 . . ?
C8 C13 H13 107.5 . . ?
C14 C13 H13 107.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C12 C16 C18 110.3(2) . . ?
C12 C16 C17 112.1(2) . . ?
C18 C16 C17 109.9(2) . . ?
C12 C16 H16 108.1 . . ?
C18 C16 H16 108.1 . . ?
C17 C16 H16 108.1 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 N2 114.3(2) . . ?
N1 C19 C20 132.1(2) . . ?
N2 C19 C20 113.6(2) . . ?
C25 C20 C21 120.1(2) . . ?
C25 C20 C19 118.6(2) . . ?
C21 C20 C19 121.1(2) . . ?
C22 C21 C20 119.2(3) . . ?
C22 C21 H21 120.4 . . ?
C20 C21 H21 120.4 . . ?
C23 C22 C21 120.5(3) . . ?
C23 C22 H22 119.8 . . ?
C21 C22 H22 119.8 . . ?
C22 C23 C24 120.4(3) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 H23 119.8 . . ?
C23 C24 C25 119.7(3) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C20 C25 C24 120.0(3) . . ?
C20 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
N2 C26 N4 105.9(2) . . ?
N2 C26 Ge1 127.11(18) . . ?
N4 C26 Ge1 126.93(18) . . ?
C28 C27 N2 106.8(2) . . ?
C28 C27 H27 126.6 . . ?
N2 C27 H27 126.6 . . ?
C27 C28 N4 106.8(2) . . ?
C27 C28 H28 126.6 . . ?
N4 C28 H28 126.6 . . ?
N3 C29 N4 113.5(2) . . ?
N3 C29 C30 131.9(2) . . ?
N4 C29 C30 114.6(2) . . ?
C31 C30 C35 119.3(2) . . ?
C31 C30 C29 119.9(2) . . ?
C35 C30 C29 120.7(2) . . ?
C32 C31 C30 120.5(3) . . ?
C32 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
C33 C32 C31 120.0(3) . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C32 C33 C34 120.1(3) . . ?
C32 C33 H33 119.9 . . ?
C34 C33 H33 119.9 . . ?
C33 C34 C35 120.5(3) . . ?
C33 C34 H34 119.7 . . ?
C35 C34 H34 119.7 . . ?
C34 C35 C30 119.6(3) . . ?
C34 C35 H35 120.2 . . ?
C30 C35 H35 120.2 . . ?
C37 C36 C41 121.6(2) . . ?
C37 C36 N3 122.6(2) . . ?
C41 C36 N3 115.7(2) . . ?
C38 C37 C36 117.4(3) . . ?
C38 C37 C42 118.9(3) . . ?
C36 C37 C42 123.6(2) . . ?
C39 C38 C37 122.0(3) . . ?
C39 C38 H38 119.0 . . ?
C37 C38 H38 119.0 . . ?
C38 C39 C40 119.4(3) . . ?
C38 C39 H39 120.3 . . ?
C40 C39 H39 120.3 . . ?
C39 C40 C41 121.8(3) . . ?
C39 C40 H40 119.1 . . ?
C41 C40 H40 119.1 . . ?
C40 C41 C36 117.7(3) . . ?
C40 C41 C45 121.2(3) . . ?
C36 C41 C45 121.0(3) . . ?
C37 C42 C43 110.3(2) . . ?
C37 C42 C44 112.0(2) . . ?
C43 C42 C44 110.5(2) . . ?
C37 C42 H42 108.0 . . ?
C43 C42 H42 108.0 . . ?
C44 C42 H42 108.0 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C47 C45 C41 110.8(3) . . ?
C47 C45 C46 110.0(3) . . ?
C41 C45 C46 113.6(3) . . ?
C47 C45 H45 107.4 . . ?
C41 C45 H45 107.4 . . ?
C46 C45 H45 107.4 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
O4 C48 C53 123.8(2) . . ?
O4 C48 C49 116.1(2) . . ?
C53 C48 C49 120.1(2) . . ?
O3 C49 C50 123.7(2) . . ?
O3 C49 C48 116.0(2) . . ?
C50 C49 C48 120.3(2) . . ?
C49 C50 C51 119.8(3) . . ?
C49 C50 Cl5 118.4(2) . . ?
C51 C50 Cl5 121.8(2) . . ?
C52 C51 C50 119.9(3) . . ?
C52 C51 Cl6 120.4(2) . . ?
C50 C51 Cl6 119.6(2) . . ?
C51 C52 C53 120.2(3) . . ?
C51 C52 Cl7 120.6(2) . . ?
C53 C52 Cl7 119.3(2) . . ?
C48 C53 C52 119.7(3) . . ?
C48 C53 Cl8 118.4(2) . . ?
C52 C53 Cl8 121.9(2) . . ?
Cl10 C54 Cl9 112.0(2) . . ?
Cl10 C54 H54A 109.2 . . ?
Cl9 C54 H54A 109.2 . . ?
Cl10 C54 H54B 109.2 . . ?
Cl9 C54 H54B 109.2 . . ?
H54A C54 H54B 107.9 . . ?
Cl12 C55 Cl11 114.5(3) . . ?
Cl12 C55 H55A 108.6 . . ?
Cl11 C55 H55A 108.6 . . ?
Cl12 C55 H55B 108.6 . . ?
Cl11 C55 H55B 108.6 . . ?
H55A C55 H55B 107.6 . . ?
 
_refine_diff_density_max    2.228
_refine_diff_density_min   -1.466
_refine_diff_density_rms    0.088



