#------------------------------------------------------------------------------
#$Date: 2019-11-08 01:24:10 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224492 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/07/7700747.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_7700747
loop_
_publ_author_name
'Leverett, Anthony R.'
'Diachenko, Vera'
'Cole, Marcus L.'
'McKay, Alasdair I.'
_publ_section_title
;
 Kinetic stabilization of low-oxidation state and terminal hydrido main
 group metal complexes by a sterically demanding
 N,N'-bis(2,6-terphenyl)triazenide.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13197
_journal_page_last               13204
_journal_paper_doi               10.1039/c9dt02562f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C48 H50 Cl Ge N3, C2 H5 O0.5'
_chemical_formula_sum            'C50 H55 Cl Ge N3 O0.5'
_chemical_formula_weight         814.01
_chemical_name_common            '[GeCl(N3Dmp2)]'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-11 deposited with the CCDC.    2019-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                102.80(4)
_cell_angle_beta                 94.73(3)
_cell_angle_gamma                111.41(4)
_cell_formula_units_Z            2
_cell_length_a                   10.637(14)
_cell_length_b                   11.483(15)
_cell_length_c                   20.41(3)
_cell_measurement_reflns_used    5190
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.27
_cell_measurement_theta_min      2.16
_cell_volume                     2226(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1126
_diffrn_reflns_av_unetI/netI     0.1424
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26484
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.485
_diffrn_reflns_theta_min         1.970
_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.3801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1593 before and 0.1025 after correction. The Ratio of minimum to maximum transmission is 0.5100. The λ/2 correction factor is 0.00150.'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_description       block
_exptl_crystal_F_000             858
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Diethyl ether'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.945
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         8105
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1764
_refine_ls_R_factor_gt           0.0892
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1258P)²+3.0149P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2165
_refine_ls_wR_factor_ref         0.2772
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4240
_reflns_number_total             8105
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt02562f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7700747--7700761.cif.'
_cod_original_formula_sum        'C50 H55 Cl Ge N3 O0.50'
_cod_database_code               7700747
_shelx_shelxl_version_number     2018/3
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C49 \\sim C49A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
3. Rigid body (RIGU) restrains
 C50, C49, C49A, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(Ge1A)=Sof(Cl1A)=1-FVAR(1)
 Sof(Ge1)=Sof(Cl1)=FVAR(1)
 Sof(H50A)=Sof(H50B)=Sof(H50C)=Sof(C49A)=Sof(H49C)=Sof(H49D)=1-FVAR(2)
 Sof(H50D)=Sof(H50E)=Sof(H50F)=Sof(C49)=Sof(H49A)=Sof(H49B)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C49A(H49C,H49D)
5.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C29(H29), C33(H33), C35(H35), C28(H28), C44(H44), C3(H3), C4(H4),
 C20(H20), C5(H5), C42(H42), C11(H11), C18(H18), C9(H9)
5.c Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C39(H39A,H39B,H39C), C46(H46A,H46B,H46C), C24(H24A,H24B,
 H24C), C38(H38A,H38B,H38C), C15(H15A,H15B,H15C), C22(H22A,H22B,H22C), C37(H37A,
 H37B,H37C), C13(H13A,H13B,H13C), C23(H23A,H23B,H23C), C47(H47A,H47B,H47C),
 C14(H14A,H14B,H14C), C50(H50D,H50E,H50F), C50(H50A,H50B,H50C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
N3 N 0.7770(4) 0.4157(4) 0.2832(2) 0.0236(10) Uani 1 1 d . . . . .
N1 N 0.6553(4) 0.5227(4) 0.2798(2) 0.0273(11) Uani 1 1 d . . . . .
N2 N 0.7394(4) 0.4820(4) 0.2462(2) 0.0287(11) Uani 1 1 d . . . . .
C40 C 1.0227(5) 0.5655(5) 0.2251(3) 0.0263(13) Uani 1 1 d . . . . .
C1 C 0.5702(5) 0.5745(5) 0.2498(3) 0.0287(13) Uani 1 1 d . . . . .
C26 C 0.8751(5) 0.2594(5) 0.2899(3) 0.0256(12) Uani 1 1 d . . . . .
C2 C 0.5293(5) 0.6592(5) 0.2982(3) 0.0287(13) Uani 1 1 d . . . . .
C25 C 0.8837(5) 0.3731(5) 0.2701(3) 0.0251(12) Uani 1 1 d . . . . .
C30 C 0.9991(5) 0.4401(5) 0.2430(3) 0.0268(12) Uani 1 1 d . . . . .
C16 C 0.5530(5) 0.4539(5) 0.1251(3) 0.0318(13) Uani 1 1 d . . . . .
C32 C 0.6312(6) 0.1026(5) 0.2797(3) 0.0296(13) Uani 1 1 d . . . . .
C27 C 0.9773(6) 0.2121(5) 0.2805(3) 0.0336(14) Uani 1 1 d . . . . .
H27 H 0.969686 0.134871 0.292643 0.040 Uiso 1 1 calc R . . . .
C31 C 0.7565(5) 0.1908(5) 0.3221(3) 0.0267(12) Uani 1 1 d . . . . .
C29 C 1.0993(5) 0.3886(5) 0.2354(3) 0.0298(13) Uani 1 1 d . . . . .
H29 H 1.176642 0.432214 0.216993 0.036 Uiso 1 1 calc R . . . .
C45 C 1.0222(5) 0.5698(5) 0.1569(3) 0.0319(14) Uani 1 1 d . . . . .
C7 C 0.5894(6) 0.7002(5) 0.3727(3) 0.0309(13) Uani 1 1 d . . . . .
C33 C 0.5237(6) 0.0372(5) 0.3103(3) 0.0316(13) Uani 1 1 d . . . . .
H33 H 0.437118 -0.018924 0.282518 0.038 Uiso 1 1 calc R . . . .
C21 C 0.6435(6) 0.5066(6) 0.0826(3) 0.0358(14) Uani 1 1 d . . . . .
C6 C 0.5197(5) 0.5437(5) 0.1795(3) 0.0297(13) Uani 1 1 d . . . . .
C41 C 1.0560(5) 0.6827(5) 0.2776(3) 0.0333(14) Uani 1 1 d . . . . .
O1 O 1.000000 1.000000 0.000000 0.084(2) Uani 1 2 d S TU P . .
C35 C 0.6656(6) 0.1411(5) 0.4214(3) 0.0350(14) Uani 1 1 d . . . . .
H35 H 0.676599 0.154519 0.469473 0.042 Uiso 1 1 calc R . . . .
C28 C 1.0910(6) 0.2763(5) 0.2535(3) 0.0339(14) Uani 1 1 d . . . . .
H28 H 1.161083 0.244165 0.247589 0.041 Uiso 1 1 calc R . . . .
C44 C 1.0522(6) 0.6890(6) 0.1414(3) 0.0429(16) Uani 1 1 d . . . . .
H44 H 1.049550 0.691015 0.095080 0.051 Uiso 1 1 calc R . . . .
C17 C 0.4911(6) 0.3195(5) 0.1136(3) 0.0391(15) Uani 1 1 d . . . . .
C3 C 0.4351(6) 0.7050(5) 0.2736(3) 0.0363(15) Uani 1 1 d . . . . .
H3 H 0.403732 0.757192 0.305484 0.044 Uiso 1 1 calc R . . . .
C36 C 0.7742(6) 0.2100(5) 0.3929(3) 0.0338(14) Uani 1 1 d . . . . .
C12 C 0.5144(6) 0.6487(5) 0.4201(3) 0.0351(14) Uani 1 1 d . . . . .
C4 C 0.3853(6) 0.6770(5) 0.2044(3) 0.0378(15) Uani 1 1 d . . . . .
H4 H 0.323442 0.711486 0.188845 0.045 Uiso 1 1 calc R . . . .
C20 C 0.6685(6) 0.4200(6) 0.0300(3) 0.0431(16) Uani 1 1 d . . . . .
H20 H 0.728835 0.454750 0.000944 0.052 Uiso 1 1 calc R . . . .
C34 C 0.5409(6) 0.0528(5) 0.3802(3) 0.0340(14) Uani 1 1 d . . . . .
C5 C 0.4291(6) 0.5970(5) 0.1586(3) 0.0376(15) Uani 1 1 d . . . . .
H5 H 0.396031 0.577636 0.111122 0.045 Uiso 1 1 calc R . . . .
C8 C 0.7229(6) 0.7980(5) 0.3964(3) 0.0416(15) Uani 1 1 d . . . . .
C48 C 0.9902(7) 0.4473(6) 0.1004(3) 0.0476(17) Uani 1 1 d . . . . .
H48A H 1.066342 0.418978 0.103806 0.071 Uiso 1 1 calc GR . . . .
H48B H 0.977554 0.464848 0.055983 0.071 Uiso 1 1 calc GR . . . .
H48C H 0.905902 0.378820 0.104801 0.071 Uiso 1 1 calc GR . . . .
C43 C 1.0858(6) 0.8042(6) 0.1918(4) 0.0474(18) Uani 1 1 d . . . . .
C19 C 0.6092(7) 0.2868(6) 0.0186(3) 0.0449(16) Uani 1 1 d . . . . .
C39 C 0.4235(6) -0.0253(6) 0.4112(3) 0.0457(17) Uani 1 1 d . . . . .
H39A H 0.338941 -0.066714 0.376974 0.069 Uiso 1 1 calc GR . . . .
H39B H 0.410502 0.032883 0.450630 0.069 Uiso 1 1 calc GR . . . .
H39C H 0.445697 -0.092234 0.425973 0.069 Uiso 1 1 calc GR . . . .
C46 C 1.0593(6) 0.6827(5) 0.3516(3) 0.0435(16) Uani 1 1 d . . . . .
H46A H 0.965706 0.655612 0.361218 0.065 Uiso 1 1 calc GR . . . .
H46B H 1.115361 0.770391 0.380714 0.065 Uiso 1 1 calc GR . . . .
H46C H 1.099124 0.622116 0.360974 0.065 Uiso 1 1 calc GR . . . .
C42 C 1.0865(6) 0.7981(5) 0.2587(4) 0.0437(16) Uani 1 1 d . . . . .
H42 H 1.108880 0.876417 0.293505 0.052 Uiso 1 1 calc R . . . .
C11 C 0.5737(7) 0.6902(6) 0.4888(3) 0.0456(16) Uani 1 1 d . . . . .
H11 H 0.521661 0.654011 0.520382 0.055 Uiso 1 1 calc R . . . .
C24 C 0.7099(6) 0.6517(6) 0.0923(3) 0.0494(17) Uani 1 1 d . . . . .
H24A H 0.640147 0.683055 0.078844 0.074 Uiso 1 1 calc GR . . . .
H24B H 0.780838 0.670859 0.063947 0.074 Uiso 1 1 calc GR . . . .
H24C H 0.751701 0.695365 0.140438 0.074 Uiso 1 1 calc GR . . . .
C38 C 0.6092(7) 0.0784(6) 0.2029(3) 0.0465(17) Uani 1 1 d . . . . .
H38A H 0.633992 0.161480 0.191501 0.070 Uiso 1 1 calc GR . . . .
H38B H 0.512443 0.023646 0.183581 0.070 Uiso 1 1 calc GR . . . .
H38C H 0.666767 0.034251 0.184002 0.070 Uiso 1 1 calc GR . . . .
C15 C 0.3670(6) 0.5483(7) 0.3980(3) 0.0520(18) Uani 1 1 d . . . . .
H15A H 0.306583 0.590213 0.385678 0.078 Uiso 1 1 calc GR . . . .
H15B H 0.337949 0.510757 0.435623 0.078 Uiso 1 1 calc GR . . . .
H15C H 0.361660 0.479280 0.358348 0.078 Uiso 1 1 calc GR . . . .
C18 C 0.5196(6) 0.2377(6) 0.0610(3) 0.0457(16) Uani 1 1 d . . . . .
H18 H 0.476738 0.146316 0.053852 0.055 Uiso 1 1 calc R . . . .
C9 C 0.7785(7) 0.8361(6) 0.4659(4) 0.0557(19) Uani 1 1 d . . . . .
H9 H 0.868975 0.900916 0.481477 0.067 Uiso 1 1 calc R . . . .
C22 C 0.3865(7) 0.2604(6) 0.1564(4) 0.058(2) Uani 1 1 d . . . . .
H22A H 0.433915 0.275378 0.202666 0.087 Uiso 1 1 calc GR . . . .
H22B H 0.338487 0.166706 0.135340 0.087 Uiso 1 1 calc GR . . . .
H22C H 0.319892 0.301105 0.158759 0.087 Uiso 1 1 calc GR . . . .
C37 C 0.9094(6) 0.3014(7) 0.4398(3) 0.0540(19) Uani 1 1 d . . . . .
H37A H 0.972390 0.256969 0.440040 0.081 Uiso 1 1 calc GR . . . .
H37B H 0.892726 0.327621 0.486266 0.081 Uiso 1 1 calc GR . . . .
H37C H 0.950084 0.378611 0.423422 0.081 Uiso 1 1 calc GR . . . .
C10 C 0.7066(8) 0.7827(7) 0.5129(4) 0.0533(18) Uani 1 1 d . . . . .
C13 C 0.8031(7) 0.8630(6) 0.3466(4) 0.0571(19) Uani 1 1 d . . . . .
H13A H 0.814061 0.797017 0.310603 0.086 Uiso 1 1 calc GR . . . .
H13B H 0.893657 0.927012 0.371196 0.086 Uiso 1 1 calc GR . . . .
H13C H 0.752932 0.906582 0.326185 0.086 Uiso 1 1 calc GR . . . .
C23 C 0.6391(9) 0.1967(7) -0.0385(4) 0.071(2) Uani 1 1 d . . . . .
H23A H 0.590077 0.192199 -0.082408 0.107 Uiso 1 1 calc GR . . . .
H23B H 0.608519 0.109612 -0.031401 0.107 Uiso 1 1 calc GR . . . .
H23C H 0.737997 0.229875 -0.038635 0.107 Uiso 1 1 calc GR . . . .
C47 C 1.1191(8) 0.9334(7) 0.1736(5) 0.078(3) Uani 1 1 d . . . . .
H47A H 1.164526 0.932358 0.133729 0.117 Uiso 1 1 calc GR . . . .
H47B H 1.180076 1.004934 0.212375 0.117 Uiso 1 1 calc GR . . . .
H47C H 1.033907 0.945562 0.163001 0.117 Uiso 1 1 calc GR . . . .
C14 C 0.7725(9) 0.8234(8) 0.5881(4) 0.080(3) Uani 1 1 d . . . . .
H14A H 0.704742 0.831043 0.616644 0.120 Uiso 1 1 calc GR . . . .
H14B H 0.850523 0.907395 0.598338 0.120 Uiso 1 1 calc GR . . . .
H14C H 0.804540 0.757833 0.597481 0.120 Uiso 1 1 calc GR . . . .
C50 C 0.8457(14) 1.0527(13) 0.0691(7) 0.142(5) Uani 1 1 d . U . . .
H50D H 0.769941 1.006059 0.030108 0.213 Uiso 0.524(15) 1 calc GR . . A 2
H50E H 0.830874 1.125968 0.097284 0.213 Uiso 0.524(15) 1 calc GR . . A 2
H50F H 0.849611 0.993617 0.096531 0.213 Uiso 0.524(15) 1 calc GR . . A 2
H50A H 0.752494 1.044733 0.053651 0.213 Uiso 0.476(15) 1 calc GR . . A 1
H50B H 0.911014 1.141386 0.073469 0.213 Uiso 0.476(15) 1 calc GR . . A 1
H50C H 0.851007 1.033780 0.113542 0.213 Uiso 0.476(15) 1 calc GR . . A 1
C49 C 0.965(2) 1.0976(19) 0.0463(10) 0.096(6) Uani 0.524(15) 1 d . U . A 2
H49A H 1.040400 1.142978 0.086385 0.116 Uiso 0.524(15) 1 calc R . . A 2
H49B H 0.962361 1.162892 0.022299 0.116 Uiso 0.524(15) 1 calc R . . A 2
C49A C 0.879(2) 0.962(2) 0.0203(10) 0.095(7) Uani 0.476(15) 1 d . U . A 1
H49C H 0.870395 0.888322 0.039478 0.114 Uiso 0.476(15) 1 calc R . . A 1
H49D H 0.806902 0.928111 -0.021049 0.114 Uiso 0.476(15) 1 calc R . . A 1
Ge1A Ge 0.6842(3) 0.4704(3) 0.36385(12) 0.0436(7) Uani 0.476(4) 1 d . . . B 2
Ge1 Ge 0.6375(2) 0.3975(3) 0.34696(11) 0.0407(6) Uani 0.524(4) 1 d . . . B 1
Cl1 Cl 0.7878(4) 0.5284(3) 0.44023(16) 0.0550(12) Uani 0.524(4) 1 d . . . B 1
Cl1A Cl 0.4754(4) 0.3127(4) 0.3338(2) 0.0631(14) Uani 0.476(4) 1 d . . . B 2
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
N2 N3 C25 122.0(4) . .
N2 N3 Ge1A 93.8(3) . .
N2 N3 Ge1 100.1(3) . .
C25 N3 Ge1A 140.3(3) . .
C25 N3 Ge1 137.8(3) . .
N2 N1 C1 122.1(4) . .
N2 N1 Ge1A 98.7(3) . .
N2 N1 Ge1 93.7(3) . .
C1 N1 Ge1A 139.0(3) . .
C1 N1 Ge1 136.8(3) . .
N3 N2 N1 104.7(4) . .
C45 C40 C30 120.0(5) . .
C45 C40 C41 119.5(5) . .
C41 C40 C30 120.3(5) . .
N1 C1 C2 114.3(5) . .
C6 C1 N1 125.5(5) . .
C6 C1 C2 120.0(5) . .
C25 C26 C31 120.4(5) . .
C27 C26 C25 119.9(4) . .
C27 C26 C31 119.6(4) . .
C1 C2 C7 120.7(5) . .
C3 C2 C1 118.2(5) . .
C3 C2 C7 121.0(5) . .
N3 C25 C26 115.9(4) . .
N3 C25 C30 124.2(4) . .
C30 C25 C26 119.8(5) . .
C25 C30 C40 124.0(5) . .
C29 C30 C40 118.3(4) . .
C29 C30 C25 117.7(5) . .
C21 C16 C6 119.1(5) . .
C17 C16 C21 119.6(5) . .
C17 C16 C6 121.2(5) . .
C31 C32 C38 122.1(4) . .
C33 C32 C31 118.5(5) . .
C33 C32 C38 119.4(5) . .
C26 C27 H27 119.5 . .
C26 C27 C28 121.0(5) . .
C28 C27 H27 119.5 . .
C32 C31 C26 119.2(5) . .
C36 C31 C26 119.9(5) . .
C36 C31 C32 120.7(4) . .
C30 C29 H29 118.4 . .
C28 C29 C30 123.1(5) . .
C28 C29 H29 118.4 . .
C40 C45 C48 120.6(5) . .
C44 C45 C40 119.3(5) . .
C44 C45 C48 120.1(5) . .
C12 C7 C2 121.8(5) . .
C12 C7 C8 118.9(6) . .
C8 C7 C2 119.2(5) . .
C32 C33 H33 119.3 . .
C34 C33 C32 121.3(5) . .
C34 C33 H33 119.3 . .
C16 C21 C24 121.1(5) . .
C20 C21 C16 118.1(5) . .
C20 C21 C24 120.8(5) . .
C1 C6 C16 124.3(5) . .
C5 C6 C1 118.4(5) . .
C5 C6 C16 117.3(5) . .
C40 C41 C46 121.2(5) . .
C42 C41 C40 118.1(6) . .
C42 C41 C46 120.6(5) . .
C49 O1 C49 180.0 2_775 .
C49A O1 C49 61.0(11) 2_775 2_775
C49A O1 C49 119.0(11) . 2_775
C49A O1 C49A 180.0 2_775 .
C36 C35 H35 119.5 . .
C36 C35 C34 121.0(5) . .
C34 C35 H35 119.5 . .
C27 C28 H28 120.8 . .
C29 C28 C27 118.5(5) . .
C29 C28 H28 120.8 . .
C45 C44 H44 119.0 . .
C43 C44 C45 122.0(6) . .
C43 C44 H44 119.0 . .
C16 C17 C22 120.3(5) . .
C18 C17 C16 120.2(5) . .
C18 C17 C22 119.4(5) . .
C2 C3 H3 118.7 . .
C4 C3 C2 122.6(5) . .
C4 C3 H3 118.7 . .
C31 C36 C37 122.1(5) . .
C35 C36 C31 119.1(5) . .
C35 C36 C37 118.8(5) . .
C7 C12 C15 121.2(5) . .
C11 C12 C7 119.9(6) . .
C11 C12 C15 118.9(5) . .
C3 C4 H4 121.0 . .
C3 C4 C5 117.9(5) . .
C5 C4 H4 121.0 . .
C21 C20 H20 118.6 . .
C19 C20 C21 122.9(5) . .
C19 C20 H20 118.6 . .
C33 C34 C35 119.2(5) . .
C33 C34 C39 119.8(5) . .
C35 C34 C39 120.9(5) . .
C6 C5 H5 118.6 . .
C4 C5 C6 122.8(6) . .
C4 C5 H5 118.6 . .
C7 C8 C13 120.1(6) . .
C9 C8 C7 119.1(6) . .
C9 C8 C13 120.9(6) . .
C45 C48 H48A 109.5 . .
C45 C48 H48B 109.5 . .
C45 C48 H48C 109.5 . .
H48A C48 H48B 109.5 . .
H48A C48 H48C 109.5 . .
H48B C48 H48C 109.5 . .
C44 C43 C47 121.0(7) . .
C42 C43 C44 117.8(5) . .
C42 C43 C47 121.2(7) . .
C20 C19 C18 117.7(5) . .
C20 C19 C23 121.3(6) . .
C18 C19 C23 120.9(6) . .
C34 C39 H39A 109.5 . .
C34 C39 H39B 109.5 . .
C34 C39 H39C 109.5 . .
H39A C39 H39B 109.5 . .
H39A C39 H39C 109.5 . .
H39B C39 H39C 109.5 . .
C41 C46 H46A 109.5 . .
C41 C46 H46B 109.5 . .
C41 C46 H46C 109.5 . .
H46A C46 H46B 109.5 . .
H46A C46 H46C 109.5 . .
H46B C46 H46C 109.5 . .
C41 C42 H42 118.4 . .
C43 C42 C41 123.2(6) . .
C43 C42 H42 118.4 . .
C12 C11 H11 119.0 . .
C10 C11 C12 122.1(6) . .
C10 C11 H11 119.0 . .
C21 C24 H24A 109.5 . .
C21 C24 H24B 109.5 . .
C21 C24 H24C 109.5 . .
H24A C24 H24B 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
C32 C38 H38A 109.5 . .
C32 C38 H38B 109.5 . .
C32 C38 H38C 109.5 . .
H38A C38 H38B 109.5 . .
H38A C38 H38C 109.5 . .
H38B C38 H38C 109.5 . .
C12 C15 H15A 109.5 . .
C12 C15 H15B 109.5 . .
C12 C15 H15C 109.5 . .
H15A C15 H15B 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C17 C18 H18 119.2 . .
C19 C18 C17 121.5(6) . .
C19 C18 H18 119.2 . .
C8 C9 H9 118.8 . .
C10 C9 C8 122.4(6) . .
C10 C9 H9 118.8 . .
C17 C22 H22A 109.5 . .
C17 C22 H22B 109.5 . .
C17 C22 H22C 109.5 . .
H22A C22 H22B 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C36 C37 H37A 109.5 . .
C36 C37 H37B 109.5 . .
C36 C37 H37C 109.5 . .
H37A C37 H37B 109.5 . .
H37A C37 H37C 109.5 . .
H37B C37 H37C 109.5 . .
C11 C10 C14 121.5(7) . .
C9 C10 C11 117.6(6) . .
C9 C10 C14 120.9(7) . .
C8 C13 H13A 109.5 . .
C8 C13 H13B 109.5 . .
C8 C13 H13C 109.5 . .
H13A C13 H13B 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C19 C23 H23A 109.5 . .
C19 C23 H23B 109.5 . .
C19 C23 H23C 109.5 . .
H23A C23 H23B 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
C43 C47 H47A 109.5 . .
C43 C47 H47B 109.5 . .
C43 C47 H47C 109.5 . .
H47A C47 H47B 109.5 . .
H47A C47 H47C 109.5 . .
H47B C47 H47C 109.5 . .
C10 C14 H14A 109.5 . .
C10 C14 H14B 109.5 . .
C10 C14 H14C 109.5 . .
H14A C14 H14B 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
H50D C50 H50E 109.5 . .
H50D C50 H50F 109.5 . .
H50E C50 H50F 109.5 . .
H50A C50 H50B 109.5 . .
H50A C50 H50C 109.5 . .
H50B C50 H50C 109.5 . .
C49 C50 H50D 109.5 . .
C49 C50 H50E 109.5 . .
C49 C50 H50F 109.5 . .
C49A C50 H50A 109.5 . .
C49A C50 H50B 109.5 . .
C49A C50 H50C 109.5 . .
O1 C49 H49A 108.2 . .
O1 C49 H49B 108.2 . .
C50 C49 O1 116.5(15) . .
C50 C49 H49A 108.2 . .
C50 C49 H49B 108.2 . .
H49A C49 H49B 107.3 . .
O1 C49A C50 120.4(17) . .
O1 C49A H49C 107.2 . .
O1 C49A H49D 107.2 . .
C50 C49A H49C 107.2 . .
C50 C49A H49D 107.2 . .
H49C C49A H49D 106.9 . .
N3 Ge1A Cl1A 101.2(2) . .
N1 Ge1A N3 61.96(19) . .
N1 Ge1A Cl1A 90.0(2) . .
N3 Ge1 N1 59.55(17) . .
N3 Ge1 Cl1 95.7(2) . .
N1 Ge1 Cl1 103.1(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N3 N2 1.318(6) .
N3 C25 1.413(7) .
N3 Ge1A 2.084(5) .
N3 Ge1 2.038(4) .
N1 N2 1.324(6) .
N1 C1 1.417(7) .
N1 Ge1A 1.976(5) .
N1 Ge1 2.168(5) .
C40 C30 1.502(7) .
C40 C45 1.404(8) .
C40 C41 1.427(8) .
C1 C2 1.437(7) .
C1 C6 1.409(8) .
C26 C25 1.424(7) .
C26 C27 1.391(8) .
C26 C31 1.512(7) .
C2 C7 1.499(8) .
C2 C3 1.396(8) .
C25 C30 1.419(7) .
C30 C29 1.399(7) .
C16 C21 1.409(7) .
C16 C6 1.499(8) .
C16 C17 1.395(8) .
C32 C31 1.410(8) .
C32 C33 1.399(7) .
C32 C38 1.512(8) .
C27 H27 0.9500 .
C27 C28 1.396(7) .
C31 C36 1.399(8) .
C29 H29 0.9500 .
C29 C28 1.393(7) .
C45 C44 1.401(8) .
C45 C48 1.513(8) .
C7 C12 1.400(8) .
C7 C8 1.412(8) .
C33 H33 0.9500 .
C33 C34 1.386(8) .
C21 C20 1.407(8) .
C21 C24 1.513(8) .
C6 C5 1.401(8) .
C41 C46 1.508(9) .
C41 C42 1.394(8) .
O1 C49 1.475(18) 2_775
O1 C49 1.475(18) .
O1 C49A 1.33(2) 2_775
O1 C49A 1.33(2) .
C35 H35 0.9500 .
C35 C36 1.395(7) .
C35 C34 1.397(8) .
C28 H28 0.9500 .
C44 H44 0.9500 .
C44 C43 1.388(9) .
C17 C18 1.393(8) .
C17 C22 1.528(8) .
C3 H3 0.9500 .
C3 C4 1.389(8) .
C36 C37 1.520(8) .
C12 C11 1.390(9) .
C12 C15 1.525(8) .
C4 H4 0.9500 .
C4 C5 1.393(8) .
C20 H20 0.9500 .
C20 C19 1.380(9) .
C34 C39 1.526(7) .
C5 H5 0.9500 .
C8 C9 1.397(10) .
C8 C13 1.525(9) .
C48 H48A 0.9800 .
C48 H48B 0.9800 .
C48 H48C 0.9800 .
C43 C42 1.381(9) .
C43 C47 1.533(8) .
C19 C18 1.390(9) .
C19 C23 1.517(9) .
C39 H39A 0.9800 .
C39 H39B 0.9800 .
C39 H39C 0.9800 .
C46 H46A 0.9800 .
C46 H46B 0.9800 .
C46 H46C 0.9800 .
C42 H42 0.9500 .
C11 H11 0.9500 .
C11 C10 1.388(9) .
C24 H24A 0.9800 .
C24 H24B 0.9800 .
C24 H24C 0.9800 .
C38 H38A 0.9800 .
C38 H38B 0.9800 .
C38 H38C 0.9800 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C18 H18 0.9500 .
C9 H9 0.9500 .
C9 C10 1.386(10) .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C37 H37A 0.9800 .
C37 H37B 0.9800 .
C37 H37C 0.9800 .
C10 C14 1.527(10) .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C23 H23A 0.9800 .
C23 H23B 0.9800 .
C23 H23C 0.9800 .
C47 H47A 0.9800 .
C47 H47B 0.9800 .
C47 H47C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C50 H50D 0.9800 .
C50 H50E 0.9800 .
C50 H50F 0.9800 .
C50 H50A 0.9800 .
C50 H50B 0.9800 .
C50 H50C 0.9800 .
C50 C49 1.35(2) .
C50 C49A 1.44(2) .
C49 H49A 0.9900 .
C49 H49B 0.9900 .
C49A H49C 0.9900 .
C49A H49D 0.9900 .
Ge1A Cl1A 2.222(6) .
Ge1 Cl1 2.216(5) .
