#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/85/4118565.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_4118565
loop_
_publ_author_name
'Saskia Stegmaier'
'Markus Waibel'
'Alexander Henze'
'Laura-Alice Jantke'
'Antti J. Karttunen'
'Thomas F. Fässler'
_publ_contact_author_address
;Department Chemie
Technische Universität München
Lichtenbergstr. 4
85747 Garching
Germany
;
_publ_contact_author_email       thomas.faessler@lrz.tu-muenchen.de
_publ_contact_author_fax         '+49 89 28913186'
_publ_contact_author_name        'Prof. Dr. Thomas F. Fässler'
_publ_contact_author_phone       '+49 89 28913134'
_publ_section_title
;
 Soluble Zintl Phases A14ZnGe16 (A= K, Rb) Featuring
 [(η3-Ge4)Zn(η2-Ge4)]6- and [Ge4]4- Clusters and the Isolation of
 [(MesCu)2(η3,η3-Ge4)]4-: The Missing Link in the Solution Chemistry of
 Tetrahedral Group 14 Element Zintl Clusters
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14450
_journal_page_last               14460
_journal_paper_doi               10.1021/ja304251t
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C42 H92.5 Cu2 Ge4 K4 N7.5 O12'
_chemical_formula_weight         1468.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing of SHELXL-97 cif-file'
_cell_angle_alpha                98.230(4)
_cell_angle_beta                 111.166(4)
_cell_angle_gamma                107.105(4)
_cell_formula_units_Z            2
_cell_length_a                   13.5093(6)
_cell_length_b                   15.8892(7)
_cell_length_c                   17.7605(8)
_cell_measurement_temperature    120(2)
_cell_volume                     3262.2(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_sigmaI/netI    0.1171
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            40591
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    2.769
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       block
_exptl_crystal_F_000             1510
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.120
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.866
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         14901
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.866
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0529P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1079
_reflns_number_gt                8614
_reflns_number_total             14901
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja304251t_si_004.cif
_cod_data_source_block           C42H92.50Cu2Ge4K4N7.50O12
_cod_original_formula_sum        'C42 H92.50 Cu2 Ge4 K4 N7.50 O12'
_cod_database_code               4118565
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cu1 Cu 1.10914(5) 0.55782(4) 0.32932(4) 0.02478(14) Uani 1 1 d .
Cu2 Cu 1.05886(5) 0.29013(4) 0.27729(4) 0.02653(14) Uani 1 1 d .
Ge1 Ge 0.99483(4) 0.40803(3) 0.21892(3) 0.02134(12) Uani 1 1 d .
Ge2 Ge 0.91793(4) 0.47279(3) 0.31933(3) 0.02256(12) Uani 1 1 d .
Ge3 Ge 0.88365(4) 0.30488(3) 0.28541(3) 0.02447(12) Uani 1 1 d .
Ge4 Ge 1.09062(4) 0.42107(3) 0.38729(3) 0.02189(12) Uani 1 1 d .
K1 K 0.71080(8) 0.37572(7) 0.11612(6) 0.0265(2) Uani 1 1 d .
K2 K 0.98083(9) 0.13420(7) 0.38077(7) 0.0327(3) Uani 1 1 d .
K3 K 0.89578(9) 0.38108(7) 0.47933(6) 0.0262(2) Uani 1 1 d .
K4 K 1.29258(12) 0.50952(12) 0.28052(11) 0.0757(5) Uani 1 1 d .
C1 C 1.1168(4) 0.1998(3) 0.2418(3) 0.0242(11) Uani 1 1 d .
C2 C 1.2340(4) 0.2110(3) 0.2794(3) 0.0251(11) Uani 1 1 d .
C3 C 1.2751(4) 0.1518(3) 0.2447(3) 0.0286(11) Uani 1 1 d .
H3 H 1.3536 0.1606 0.2724 0.034 Uiso 1 1 calc R
C4 C 1.2065(5) 0.0816(3) 0.1724(3) 0.0326(12) Uani 1 1 d .
C5 C 1.0926(5) 0.0699(3) 0.1351(3) 0.0326(12) Uani 1 1 d .
H5 H 1.0431 0.0215 0.0849 0.039 Uiso 1 1 calc R
C6 C 1.0468(4) 0.1260(3) 0.1676(3) 0.0296(11) Uani 1 1 d .
C7 C 1.3165(4) 0.2863(3) 0.3580(3) 0.0337(12) Uani 1 1 d .
H7A H 1.3467 0.2597 0.4036 0.051 Uiso 1 1 calc R
H7B H 1.2771 0.3238 0.3735 0.051 Uiso 1 1 calc R
H7C H 1.3798 0.3247 0.3483 0.051 Uiso 1 1 calc R
C8 C 1.2538(5) 0.0195(4) 0.1357(4) 0.0506(16) Uani 1 1 d .
H8A H 1.2669 0.0385 0.0889 0.076 Uiso 1 1 calc R
H8B H 1.1988 -0.0440 0.1153 0.076 Uiso 1 1 calc R
H8C H 1.3262 0.0237 0.1793 0.076 Uiso 1 1 calc R
C9 C 0.9211(4) 0.1075(4) 0.1234(3) 0.0386(13) Uani 1 1 d .
H9A H 0.8876 0.0610 0.0692 0.058 Uiso 1 1 calc R
H9B H 0.9110 0.1642 0.1138 0.058 Uiso 1 1 calc R
H9C H 0.8829 0.0852 0.1582 0.058 Uiso 1 1 calc R
C10 C 1.2177(4) 0.6788(3) 0.3408(3) 0.0248(11) Uani 1 1 d .
C11 C 1.1850(4) 0.7268(3) 0.2809(3) 0.0264(11) Uani 1 1 d .
C12 C 1.2591(4) 0.8129(3) 0.2880(3) 0.0330(12) Uani 1 1 d .
H12 H 1.2347 0.8429 0.2462 0.040 Uiso 1 1 calc R
C13 C 1.3672(5) 0.8563(3) 0.3541(4) 0.0416(14) Uani 1 1 d .
C14 C 1.4002(4) 0.8104(4) 0.4125(4) 0.0368(13) Uani 1 1 d .
H14 H 1.4743 0.8384 0.4579 0.044 Uiso 1 1 calc R
C15 C 1.3285(4) 0.7238(3) 0.4076(3) 0.0294(11) Uani 1 1 d .
C16 C 1.0669(4) 0.6864(3) 0.2093(3) 0.0327(12) Uani 1 1 d .
H16A H 1.0621 0.7236 0.1695 0.049 Uiso 1 1 calc R
H16B H 1.0100 0.6859 0.2314 0.049 Uiso 1 1 calc R
H16C H 1.0517 0.6235 0.1805 0.049 Uiso 1 1 calc R
C17 C 1.4470(5) 0.9500(4) 0.3596(4) 0.0596(18) Uani 1 1 d .
H17A H 1.4801 0.9902 0.4169 0.089 Uiso 1 1 calc R
H17B H 1.4037 0.9770 0.3199 0.089 Uiso 1 1 calc R
H17C H 1.5086 0.9429 0.3456 0.089 Uiso 1 1 calc R
C18 C 1.3703(4) 0.6816(4) 0.4771(3) 0.0398(14) Uani 1 1 d .
H18A H 1.4509 0.6914 0.4923 0.060 Uiso 1 1 calc R
H18B H 1.3247 0.6157 0.4583 0.060 Uiso 1 1 calc R
H18C H 1.3626 0.7103 0.5263 0.060 Uiso 1 1 calc R
C19 C 0.4786(5) 0.3014(4) 0.1867(4) 0.0525(17) Uani 1 1 d .
H19A H 0.4026 0.2788 0.1384 0.063 Uiso 1 1 calc R
H19B H 0.4686 0.3149 0.2391 0.063 Uiso 1 1 calc R
C20 C 0.5293(5) 0.2310(4) 0.1870(4) 0.0500(16) Uani 1 1 d .
H20A H 0.6085 0.2556 0.2318 0.060 Uiso 1 1 calc R
H20B H 0.4839 0.1768 0.1980 0.060 Uiso 1 1 calc R
C21 C 0.5785(5) 0.1391(4) 0.1020(4) 0.0453(15) Uani 1 1 d .
H21A H 0.5318 0.0820 0.1084 0.054 Uiso 1 1 calc R
H21B H 0.6567 0.1617 0.1479 0.054 Uiso 1 1 calc R
C22 C 0.5836(5) 0.1201(3) 0.0189(4) 0.0446(15) Uani 1 1 d .
H22A H 0.6093 0.0683 0.0120 0.053 Uiso 1 1 calc R
H22B H 0.5068 0.1034 -0.0273 0.053 Uiso 1 1 calc R
C23 C 0.6891(5) 0.1865(4) -0.0532(4) 0.0457(15) Uani 1 1 d .
H23A H 0.6228 0.1780 -0.1057 0.055 Uiso 1 1 calc R
H23B H 0.7077 0.1308 -0.0583 0.055 Uiso 1 1 calc R
C24 C 0.7905(5) 0.2692(4) -0.0394(4) 0.0455(15) Uani 1 1 d .
H24A H 0.8554 0.2799 0.0148 0.055 Uiso 1 1 calc R
H24B H 0.8150 0.2591 -0.0851 0.055 Uiso 1 1 calc R
C25 C 0.8515(4) 0.4276(4) -0.0219(3) 0.0394(13) Uani 1 1 d .
H25A H 0.8795 0.4218 -0.0661 0.047 Uiso 1 1 calc R
H25B H 0.9151 0.4383 0.0330 0.047 Uiso 1 1 calc R
C26 C 0.8118(5) 0.5058(4) -0.0206(3) 0.0388(13) Uani 1 1 d .
H26A H 0.8735 0.5626 -0.0140 0.047 Uiso 1 1 calc R
H26B H 0.7447 0.4931 -0.0741 0.047 Uiso 1 1 calc R
C27 C 0.7548(5) 0.5966(3) 0.0612(3) 0.0370(13) Uani 1 1 d .
H27A H 0.6844 0.5901 0.0128 0.044 Uiso 1 1 calc R
H27B H 0.8182 0.6515 0.0666 0.044 Uiso 1 1 calc R
C28 C 0.7373(5) 0.6070(3) 0.1396(3) 0.0393(13) Uani 1 1 d .
H28A H 0.8048 0.6072 0.1868 0.047 Uiso 1 1 calc R
H28B H 0.7281 0.6659 0.1539 0.047 Uiso 1 1 calc R
C29 C 0.6179(5) 0.5421(4) 0.2004(3) 0.0361(13) Uani 1 1 d .
H29A H 0.6003 0.5976 0.2110 0.043 Uiso 1 1 calc R
H29B H 0.6871 0.5483 0.2497 0.043 Uiso 1 1 calc R
C30 C 0.5186(4) 0.4583(4) 0.1878(3) 0.0408(14) Uani 1 1 d .
H30A H 0.4988 0.4656 0.2362 0.049 Uiso 1 1 calc R
H30B H 0.4507 0.4491 0.1361 0.049 Uiso 1 1 calc R
C31 C 1.2365(5) 0.0619(3) 0.4306(4) 0.0390(13) Uani 1 1 d .
H31A H 1.2351 0.0228 0.4691 0.047 Uiso 1 1 calc R
H31B H 1.3150 0.0853 0.4340 0.047 Uiso 1 1 calc R
C32 C 1.1532(5) 0.0065(3) 0.3422(3) 0.0376(13) Uani 1 1 d .
H32A H 1.1533 0.0460 0.3038 0.045 Uiso 1 1 calc R
H32B H 1.1760 -0.0437 0.3239 0.045 Uiso 1 1 calc R
C33 C 0.9628(5) -0.0888(4) 0.2582(3) 0.0380(13) Uani 1 1 d .
H33A H 0.9818 -0.1435 0.2466 0.046 Uiso 1 1 calc R
H33B H 0.9672 -0.0562 0.2154 0.046 Uiso 1 1 calc R
C34 C 0.8432(5) -0.1183(3) 0.2533(3) 0.0429(14) Uani 1 1 d .
H34A H 0.7888 -0.1657 0.1996 0.052 Uiso 1 1 calc R
H34B H 0.8406 -0.1446 0.3002 0.052 Uiso 1 1 calc R
C35 C 0.6968(5) -0.0638(4) 0.2449(4) 0.0453(15) Uani 1 1 d .
H35A H 0.6789 -0.1057 0.2785 0.054 Uiso 1 1 calc R
H35B H 0.6459 -0.0957 0.1848 0.054 Uiso 1 1 calc R
C36 C 0.6778(5) 0.0212(4) 0.2702(4) 0.0453(15) Uani 1 1 d .
H36A H 0.7068 0.0670 0.2433 0.054 Uiso 1 1 calc R
H36B H 0.5950 0.0075 0.2523 0.054 Uiso 1 1 calc R
C37 C 0.7157(4) 0.1328(3) 0.3918(4) 0.0374(14) Uani 1 1 d .
H37A H 0.6338 0.1146 0.3801 0.045 Uiso 1 1 calc R
H37B H 0.7355 0.1824 0.3656 0.045 Uiso 1 1 calc R
C38 C 0.7867(5) 0.1650(3) 0.4826(4) 0.0375(13) Uani 1 1 d .
H38A H 0.7608 0.2078 0.5095 0.045 Uiso 1 1 calc R
H38B H 0.7791 0.1123 0.5068 0.045 Uiso 1 1 calc R
C39 C 0.9779(5) 0.2371(4) 0.5851(3) 0.0365(13) Uani 1 1 d .
H39A H 0.9726 0.1824 0.6064 0.044 Uiso 1 1 calc R
H39B H 0.9556 0.2785 0.6172 0.044 Uiso 1 1 calc R
C40 C 1.0966(5) 0.2848(4) 0.5971(3) 0.0362(13) Uani 1 1 d .
H40A H 1.0999 0.3345 0.5691 0.043 Uiso 1 1 calc R
H40B H 1.1473 0.3127 0.6579 0.043 Uiso 1 1 calc R
C41 C 1.2437(4) 0.2643(4) 0.5626(3) 0.0405(14) Uani 1 1 d .
H41A H 1.2993 0.3052 0.6193 0.049 Uiso 1 1 calc R
H41B H 1.2371 0.3016 0.5222 0.049 Uiso 1 1 calc R
C42 C 1.2831(4) 0.1909(4) 0.5380(3) 0.0384(13) Uani 1 1 d .
H42A H 1.3610 0.2189 0.5414 0.046 Uiso 1 1 calc R
H42B H 1.2860 0.1520 0.5770 0.046 Uiso 1 1 calc R
N1 N 1.0000 0.0000 0.5000 0.060(2) Uani 1 2 d S
N2 N 1.2129(4) 0.3488(3) 0.1473(3) 0.0533(14) Uani 1 1 d .
N3 N 1.4099(4) 0.6682(4) 0.2374(3) 0.0567(14) Uani 1 1 d .
N4 N 1.5067(5) 0.5434(4) 0.4119(4) 0.0703(17) Uani 1 1 d .
N5 N 0.6812(4) 0.4604(4) 0.3900(3) 0.0496(13) Uani 1 1 d .
N6 N 0.5104(4) 0.6823(3) 0.0830(3) 0.0556(14) Uani 1 1 d .
N7 N 0.2896(6) 0.1632(5) 0.9578(4) 0.093(2) Uani 1 1 d .
N8 N 0.0561(6) 0.1867(4) 0.9682(4) 0.088(2) Uani 1 1 d .
O1 O 0.5528(3) 0.3823(2) 0.1807(2) 0.0403(9) Uani 1 1 d .
O2 O 0.5295(3) 0.2057(2) 0.1065(2) 0.0398(9) Uani 1 1 d .
O3 O 0.6621(3) 0.2006(2) 0.0164(2) 0.0375(9) Uani 1 1 d .
O4 O 0.7576(3) 0.3458(2) -0.0388(2) 0.0356(8) Uani 1 1 d .
O5 O 0.7815(3) 0.5172(2) 0.0480(2) 0.0329(8) Uani 1 1 d .
O6 O 0.6381(3) 0.5332(2) 0.1273(2) 0.0331(8) Uani 1 1 d .
O7 O 1.2067(3) 0.1365(2) 0.4548(2) 0.0297(8) Uani 1 1 d .
O8 O 1.0415(3) -0.0308(2) 0.3387(2) 0.0311(8) Uani 1 1 d .
O9 O 0.8125(3) -0.0401(2) 0.2585(2) 0.0360(9) Uani 1 1 d .
O10 O 0.7363(3) 0.0557(2) 0.3577(2) 0.0368(9) Uani 1 1 d .
O11 O 0.9033(3) 0.2103(2) 0.4987(2) 0.0283(8) Uani 1 1 d .
O12 O 1.1347(3) 0.2211(2) 0.5624(2) 0.0338(8) Uani 1 1 d .
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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
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
C10 Cu1 Ge2 145.38(13) . .
C10 Cu1 Ge1 136.66(14) . .
Ge2 Cu1 Ge1 63.27(2) . .
C10 Cu1 Ge4 143.49(14) . .
Ge2 Cu1 Ge4 63.86(2) . .
Ge1 Cu1 Ge4 66.39(2) . .
C10 Cu1 K4 76.54(13) . .
Ge2 Cu1 K4 136.52(4) . .
Ge1 Cu1 K4 76.43(3) . .
Ge4 Cu1 K4 86.20(4) . .
C10 Cu1 K3 95.74(13) . 2_766
Ge2 Cu1 K3 70.54(2) . 2_766
Ge1 Cu1 K3 127.48(3) . 2_766
Ge4 Cu1 K3 71.92(2) . 2_766
K4 Cu1 K3 131.33(4) . 2_766
C1 Cu2 Ge4 147.28(14) . .
C1 Cu2 Ge1 135.24(13) . .
Ge4 Cu2 Ge1 67.40(2) . .
C1 Cu2 Ge3 142.20(14) . .
Ge4 Cu2 Ge3 63.78(2) . .
Ge1 Cu2 Ge3 62.66(2) . .
C1 Cu2 K2 80.64(13) . .
Ge4 Cu2 K2 93.09(3) . .
Ge1 Cu2 K2 138.14(3) . .
Ge3 Cu2 K2 75.54(3) . .
C1 Cu2 K4 97.53(14) . .
Ge4 Cu2 K4 71.16(3) . .
Ge1 Cu2 K4 62.04(3) . .
Ge3 Cu2 K4 118.11(3) . .
K2 Cu2 K4 147.97(4) . .
Cu2 Ge1 Cu1 107.48(3) . .
Cu2 Ge1 Ge3 58.85(2) . .
Cu1 Ge1 Ge3 104.77(2) . .
Cu2 Ge1 Ge2 104.81(2) . .
Cu1 Ge1 Ge2 57.87(2) . .
Ge3 Ge1 Ge2 57.844(19) . .
Cu2 Ge1 Ge4 55.74(2) . .
Cu1 Ge1 Ge4 57.30(2) . .
Ge3 Ge1 Ge4 58.669(19) . .
Ge2 Ge1 Ge4 59.060(18) . .
Cu2 Ge1 K1 122.82(3) . .
Cu1 Ge1 K1 112.69(3) . .
Ge3 Ge1 K1 72.54(2) . .
Ge2 Ge1 K1 67.71(2) . .
Ge4 Ge1 K1 120.79(3) . .
Cu2 Ge1 K4 79.48(4) . .
Cu1 Ge1 K4 60.28(3) . .
Ge3 Ge1 K4 129.93(4) . .
Ge2 Ge1 K4 116.14(3) . .
Ge4 Ge1 K4 75.82(3) . .
K1 Ge1 K4 156.72(4) . .
Cu1 Ge2 Ge3 108.07(2) . .
Cu1 Ge2 Ge1 58.87(2) . .
Ge3 Ge2 Ge1 60.939(19) . .
Cu1 Ge2 Ge4 59.08(2) . .
Ge3 Ge2 Ge4 61.071(19) . .
Ge1 Ge2 Ge4 63.195(19) . .
Cu1 Ge2 K1 113.56(3) . .
Ge3 Ge2 K1 73.47(2) . .
Ge1 Ge2 K1 67.86(2) . .
Ge4 Ge2 K1 124.50(3) . .
Cu1 Ge2 K3 119.34(3) . .
Ge3 Ge2 K3 67.89(2) . .
Ge1 Ge2 K3 121.98(3) . .
Ge4 Ge2 K3 69.48(2) . .
K1 Ge2 K3 121.35(3) . .
Cu1 Ge2 K3 67.75(2) . 2_766
Ge3 Ge2 K3 120.96(3) . 2_766
Ge1 Ge2 K3 121.18(3) . 2_766
Ge4 Ge2 K3 69.64(2) . 2_766
K1 Ge2 K3 165.03(3) . 2_766
K3 Ge2 K3 65.86(3) . 2_766
Cu2 Ge3 Ge2 107.22(2) . .
Cu2 Ge3 Ge1 58.49(2) . .
Ge2 Ge3 Ge1 61.216(19) . .
Cu2 Ge3 Ge4 57.34(2) . .
Ge2 Ge3 Ge4 61.831(19) . .
Ge1 Ge3 Ge4 63.548(19) . .
Cu2 Ge3 K3 118.13(3) . .
Ge2 Ge3 K3 69.10(2) . .
Ge1 Ge3 K3 123.27(3) . .
Ge4 Ge3 K3 70.15(2) . .
Cu2 Ge3 K1 115.66(3) . .
Ge2 Ge3 K1 65.04(2) . .
Ge1 Ge3 K1 64.56(2) . .
Ge4 Ge3 K1 118.13(3) . .
K3 Ge3 K1 116.60(3) . .
Cu2 Ge3 K2 63.74(2) . .
Ge2 Ge3 K2 141.12(3) . .
Ge1 Ge3 K2 122.19(3) . .
Ge4 Ge3 K2 84.48(2) . .
K3 Ge3 K2 82.10(3) . .
K1 Ge3 K2 153.84(3) . .
Cu2 Ge4 Cu1 107.59(3) . .
Cu2 Ge4 Ge3 58.88(2) . .
Cu1 Ge4 Ge3 103.24(2) . .
Cu2 Ge4 Ge2 104.64(2) . .
Cu1 Ge4 Ge2 57.059(19) . .
Ge3 Ge4 Ge2 57.098(18) . .
Cu2 Ge4 Ge1 56.86(2) . .
Cu1 Ge4 Ge1 56.31(2) . .
Ge3 Ge4 Ge1 57.783(18) . .
Ge2 Ge4 Ge1 57.745(18) . .
Cu2 Ge4 K3 115.49(3) . .
Cu1 Ge4 K3 114.77(3) . .
Ge3 Ge4 K3 65.54(2) . .
Ge2 Ge4 K3 66.05(2) . .
Ge1 Ge4 K3 114.78(2) . .
Cu2 Ge4 K3 170.81(3) . 2_766
Cu1 Ge4 K3 65.93(2) . 2_766
Ge3 Ge4 K3 115.12(3) . 2_766
Ge2 Ge4 K3 66.53(2) . 2_766
Ge1 Ge4 K3 114.38(2) . 2_766
K3 Ge4 K3 64.17(3) . 2_766
Cu2 Ge4 K4 72.31(3) . .
Cu1 Ge4 K4 53.72(3) . .
Ge3 Ge4 K4 115.63(3) . .
Ge2 Ge4 K4 104.38(3) . .
Ge1 Ge4 K4 61.25(3) . .
K3 Ge4 K4 168.45(3) . .
K3 Ge4 K4 106.68(3) 2_766 .
O1 K1 O5 116.72(11) . .
O1 K1 O3 114.44(11) . .
O5 K1 O3 113.24(11) . .
O1 K1 O6 58.16(10) . .
O5 K1 O6 58.81(10) . .
O3 K1 O6 145.29(10) . .
O1 K1 O2 57.74(10) . .
O5 K1 O2 150.08(11) . .
O3 K1 O2 57.58(10) . .
O6 K1 O2 110.60(10) . .
O1 K1 O4 147.44(11) . .
O5 K1 O4 57.09(10) . .
O3 K1 O4 56.54(10) . .
O6 K1 O4 109.40(10) . .
O2 K1 O4 109.89(10) . .
O1 K1 Ge2 86.85(8) . .
O5 K1 Ge2 98.57(7) . .
O3 K1 Ge2 124.23(8) . .
O6 K1 Ge2 90.24(7) . .
O2 K1 Ge2 109.86(8) . .
O4 K1 Ge2 124.89(7) . .
O1 K1 Ge1 129.82(8) . .
O5 K1 Ge1 87.14(7) . .
O3 K1 Ge1 91.20(8) . .
O6 K1 Ge1 120.11(7) . .
O2 K1 Ge1 119.65(8) . .
O4 K1 Ge1 82.74(7) . .
Ge2 K1 Ge1 44.431(17) . .
O1 K1 C28 78.51(12) . .
O5 K1 C28 41.86(11) . .
O3 K1 C28 151.45(12) . .
O6 K1 C28 23.08(11) . .
O2 K1 C28 133.54(12) . .
O4 K1 C28 98.38(12) . .
Ge2 K1 C28 79.99(9) . .
Ge1 K1 C28 99.40(9) . .
O1 K1 Ge3 95.35(8) . .
O5 K1 Ge3 128.75(8) . .
O3 K1 Ge3 83.95(8) . .
O6 K1 Ge3 128.68(7) . .
O2 K1 Ge3 80.53(8) . .
O4 K1 Ge3 113.06(7) . .
Ge2 K1 Ge3 41.495(16) . .
Ge1 K1 Ge3 42.898(16) . .
C28 K1 Ge3 121.49(9) . .
O7 K2 O11 115.10(10) . .
O7 K2 O9 114.01(10) . .
O11 K2 O9 113.80(10) . .
O7 K2 O12 57.33(9) . .
O11 K2 O12 57.95(9) . .
O9 K2 O12 143.09(10) . .
O7 K2 O10 147.87(10) . .
O11 K2 O10 57.98(9) . .
O9 K2 O10 56.61(10) . .
O12 K2 O10 109.51(10) . .
O7 K2 O8 57.05(9) . .
O11 K2 O8 138.70(10) . .
O9 K2 O8 56.96(10) . .
O12 K2 O8 103.40(9) . .
O10 K2 O8 105.38(10) . .
O7 K2 N1 68.50(7) . .
O11 K2 N1 79.50(7) . .
O9 K2 N1 80.06(7) . .
O12 K2 N1 63.24(7) . .
O10 K2 N1 79.41(7) . .
O8 K2 N1 59.59(6) . .
O7 K2 Cu2 91.64(7) . .
O11 K2 Cu2 110.30(7) . .
O9 K2 Cu2 109.74(7) . .
O12 K2 Cu2 106.44(7) . .
O10 K2 Cu2 120.45(7) . .
O8 K2 Cu2 110.40(7) . .
N1 K2 Cu2 160.14(4) . .
O7 K2 Ge3 128.58(8) . .
O11 K2 Ge3 78.05(7) . .
O9 K2 Ge3 102.52(7) . .
O12 K2 Ge3 109.56(7) . .
O10 K2 Ge3 82.60(7) . .
O8 K2 Ge3 141.18(7) . .
N1 K2 Ge3 156.40(4) . .
Cu2 K2 Ge3 40.723(17) . .
O7 K2 K3 120.27(7) . .
O11 K2 K3 34.47(6) . .
O9 K2 K3 125.29(8) . .
O12 K2 K3 70.63(7) . .
O10 K2 K3 73.39(7) . .
O8 K2 K3 172.60(7) . .
N1 K2 K3 113.16(3) . .
Cu2 K2 K3 75.98(2) . .
Ge3 K2 K3 46.208(19) . .
O11 K3 C38 25.01(11) . .
O11 K3 C39 24.61(11) . .
C38 K3 C39 41.36(13) . .
O11 K3 Ge3 84.85(7) . .
C38 K3 Ge3 90.02(9) . .
C39 K3 Ge3 104.76(9) . .
O11 K3 Cu1 92.38(7) . 2_766
C38 K3 Cu1 86.04(9) . 2_766
C39 K3 Cu1 73.47(9) . 2_766
Ge3 K3 Cu1 175.59(4) . 2_766
O11 K3 Ge2 126.98(7) . .
C38 K3 Ge2 131.55(10) . .
C39 K3 Ge2 141.41(9) . .
Ge3 K3 Ge2 43.008(17) . .
Cu1 K3 Ge2 140.27(3) 2_766 .
O11 K3 N5 135.11(12) . .
C38 K3 N5 110.90(13) . .
C39 K3 N5 147.06(13) . .
Ge3 K3 N5 89.56(8) . .
Cu1 K3 N5 89.98(8) 2_766 .
Ge2 K3 N5 66.94(8) . .
O11 K3 Ge2 102.04(7) . 2_766
C38 K3 Ge2 111.87(10) . 2_766
C39 K3 Ge2 77.44(9) . 2_766
Ge3 K3 Ge2 142.29(3) . 2_766
Cu1 K3 Ge2 41.721(17) 2_766 2_766
Ge2 K3 Ge2 114.14(3) . 2_766
N5 K3 Ge2 109.03(8) . 2_766
O11 K3 Ge4 95.04(7) . .
C38 K3 Ge4 114.95(9) . .
C39 K3 Ge4 99.16(9) . .
Ge3 K3 Ge4 44.313(17) . .
Cu1 K3 Ge4 139.61(3) 2_766 .
Ge2 K3 Ge4 44.476(17) . .
N5 K3 Ge4 111.38(9) . .
Ge2 K3 Ge4 97.98(3) 2_766 .
O11 K3 Ge4 134.18(7) . 2_766
C38 K3 Ge4 125.95(9) . 2_766
C39 K3 Ge4 112.54(9) . 2_766
Ge3 K3 Ge4 140.89(3) . 2_766
Cu1 K3 Ge4 42.155(17) 2_766 2_766
Ge2 K3 Ge4 98.12(3) . 2_766
N5 K3 Ge4 65.26(8) . 2_766
Ge2 K3 Ge4 43.832(16) 2_766 2_766
Ge4 K3 Ge4 115.83(3) . 2_766
O11 K3 K3 137.92(8) . 2_766
C38 K3 K3 161.93(11) . 2_766
C39 K3 K3 120.79(11) . 2_766
Ge3 K3 K3 93.77(4) . 2_766
Cu1 K3 K3 90.58(4) 2_766 2_766
Ge2 K3 K3 57.75(3) . 2_766
N5 K3 K3 86.82(9) . 2_766
Ge2 K3 K3 56.39(3) 2_766 2_766
Ge4 K3 K3 58.49(3) . 2_766
Ge4 K3 K3 57.34(3) 2_766 2_766
O11 K3 K2 36.09(7) . .
C38 K3 K2 53.17(9) . .
C39 K3 K2 53.08(8) . .
Ge3 K3 K2 51.69(2) . .
Cu1 K3 K2 126.47(3) 2_766 .
Ge2 K3 K2 91.45(3) . .
N5 K3 K2 133.00(8) . .
Ge2 K3 K2 117.94(3) 2_766 .
Ge4 K3 K2 61.79(2) . .
Ge4 K3 K2 161.73(3) 2_766 .
K3 K3 K2 117.22(4) 2_766 .
N4 K4 N2 113.91(16) . .
N4 K4 N3 86.95(17) . .
N2 K4 N3 109.07(14) . .
N4 K4 Cu1 117.68(12) . .
N2 K4 Cu1 117.65(11) . .
N3 K4 Cu1 106.28(11) . .
N4 K4 C10 104.60(14) . .
N2 K4 C10 141.48(14) . .
N3 K4 C10 72.73(12) . .
Cu1 K4 C10 35.46(8) . .
N4 K4 Ge1 142.40(14) . .
N2 K4 Ge1 74.44(10) . .
N3 K4 Ge1 126.48(12) . .
Cu1 K4 Ge1 43.29(2) . .
C10 K4 Ge1 74.70(8) . .
N4 K4 Ge4 100.22(14) . .
N2 K4 Ge4 99.48(10) . .
N3 K4 Ge4 144.75(10) . .
Cu1 K4 Ge4 40.07(2) . .
C10 K4 Ge4 72.06(8) . .
Ge1 K4 Ge4 42.93(2) . .
N4 K4 Cu2 109.98(14) . .
N2 K4 Cu2 63.21(10) . .
N3 K4 Cu2 162.99(12) . .
Cu1 K4 Cu2 68.01(3) . .
C10 K4 Cu2 103.44(8) . .
Ge1 K4 Cu2 38.48(2) . .
Ge4 K4 Cu2 36.529(19) . .
C6 C1 C2 115.3(4) . .
C6 C1 Cu2 120.9(3) . .
C2 C1 Cu2 123.1(3) . .
C3 C2 C1 121.3(4) . .
C3 C2 C7 118.3(4) . .
C1 C2 C7 120.4(4) . .
C4 C3 C2 122.6(5) . .
C3 C4 C5 116.9(4) . .
C3 C4 C8 121.3(5) . .
C5 C4 C8 121.8(5) . .
C4 C5 C6 122.9(5) . .
C5 C6 C1 121.0(5) . .
C5 C6 C9 119.3(5) . .
C1 C6 C9 119.6(4) . .
C11 C10 C15 116.0(4) . .
C11 C10 Cu1 119.8(3) . .
C15 C10 Cu1 124.2(4) . .
C11 C10 K4 115.4(3) . .
C15 C10 K4 90.0(3) . .
Cu1 C10 K4 68.00(13) . .
C12 C11 C10 121.2(5) . .
C12 C11 C16 118.8(5) . .
C10 C11 C16 120.1(4) . .
C13 C12 C11 122.2(5) . .
C14 C13 C12 117.3(5) . .
C14 C13 C17 121.7(6) . .
C12 C13 C17 121.0(6) . .
C13 C14 C15 122.4(5) . .
C14 C15 C10 121.0(5) . .
C14 C15 C18 118.1(5) . .
C10 C15 C18 120.8(4) . .
O1 C19 C20 108.8(5) . .
O2 C20 C19 108.0(5) . .
O2 C21 C22 109.2(5) . .
O3 C22 C21 108.0(4) . .
O3 C23 C24 108.4(4) . .
O4 C24 C23 108.2(4) . .
O4 C25 C26 108.4(4) . .
O5 C26 C25 108.5(4) . .
O5 C27 C28 108.4(4) . .
O6 C28 C27 109.3(4) . .
O6 C28 K1 54.7(2) . .
C27 C28 K1 85.1(3) . .
O6 C29 C30 109.0(4) . .
O1 C30 C29 107.3(4) . .
O7 C31 C32 109.5(4) . .
O8 C32 C31 109.4(4) . .
O8 C33 C34 109.7(4) . .
O9 C34 C33 108.4(4) . .
O9 C35 C36 108.8(4) . .
O10 C36 C35 108.0(5) . .
O10 C37 C38 108.3(4) . .
O11 C38 C37 109.5(4) . .
O11 C38 K3 56.5(2) . .
C37 C38 K3 93.0(3) . .
O11 C39 C40 109.4(4) . .
O11 C39 K3 55.8(2) . .
C40 C39 K3 89.7(3) . .
O12 C40 C39 109.6(4) . .
O12 C41 C42 107.9(4) . .
O7 C42 C41 109.5(4) . .
K2 N1 K2 180.0 2_756 .
C30 O1 C19 114.2(4) . .
C30 O1 K1 122.4(3) . .
C19 O1 K1 121.2(3) . .
C21 O2 C20 111.6(4) . .
C21 O2 K1 102.6(3) . .
C20 O2 K1 100.6(3) . .
C23 O3 C22 113.2(4) . .
C23 O3 K1 123.7(3) . .
C22 O3 K1 121.4(3) . .
C24 O4 C25 111.1(4) . .
C24 O4 K1 105.4(3) . .
C25 O4 K1 103.6(3) . .
C26 O5 C27 113.3(4) . .
C26 O5 K1 123.7(3) . .
C27 O5 K1 120.2(3) . .
C29 O6 C28 110.6(4) . .
C29 O6 K1 105.7(3) . .
C28 O6 K1 102.2(3) . .
C42 O7 C31 111.6(4) . .
C42 O7 K2 120.7(3) . .
C31 O7 K2 122.9(3) . .
C33 O8 C32 110.9(4) . .
C33 O8 K2 110.8(3) . .
C32 O8 K2 105.1(3) . .
C35 O9 C34 111.8(4) . .
C35 O9 K2 118.3(3) . .
C34 O9 K2 119.2(3) . .
C36 O10 C37 114.0(4) . .
C36 O10 K2 101.3(3) . .
C37 O10 K2 104.6(3) . .
C39 O11 C38 112.4(4) . .
C39 O11 K3 99.6(3) . .
C38 O11 K3 98.5(3) . .
C39 O11 K2 116.9(3) . .
C38 O11 K2 116.6(3) . .
K3 O11 K2 109.44(11) . .
C40 O12 C41 112.7(4) . .
C40 O12 K2 110.1(3) . .
C41 O12 K2 103.1(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 C10 1.975(5) .
Cu1 Ge2 2.4652(7) .
Cu1 Ge1 2.4918(8) .
Cu1 Ge4 2.5201(7) .
Cu1 K4 3.1560(14) .
Cu1 K3 3.4284(12) 2_766
Cu2 C1 1.956(4) .
Cu2 Ge4 2.4567(7) .
Cu2 Ge1 2.4888(7) .
Cu2 Ge3 2.4983(7) .
Cu2 K2 3.4341(13) .
Cu2 K4 3.9321(18) .
Ge1 Ge3 2.5930(7) .
Ge1 Ge2 2.6000(7) .
Ge1 Ge4 2.7441(7) .
Ge1 K1 3.4401(11) .
Ge1 K4 3.5324(15) .
Ge2 Ge3 2.5114(7) .
Ge2 Ge4 2.6369(7) .
Ge2 K1 3.4364(12) .
Ge2 K3 3.4397(11) .
Ge2 K3 3.4926(12) 2_766
Ge3 Ge4 2.6180(7) .
Ge3 K3 3.4112(11) .
Ge3 K1 3.6339(12) .
Ge3 K2 3.7081(12) .
Ge4 K3 3.5249(11) .
Ge4 K3 3.5696(11) 2_766
Ge4 K4 3.9062(17) .
K1 O1 2.784(3) .
K1 O5 2.789(3) .
K1 O3 2.826(3) .
K1 O6 2.951(3) .
K1 O2 3.000(4) .
K1 O4 3.043(3) .
K1 C28 3.533(5) .
K2 O7 2.840(3) .
K2 O11 2.924(3) .
K2 O9 2.927(3) .
K2 O12 2.972(3) .
K2 O10 3.015(4) .
K2 O8 3.041(3) .
K2 N1 3.2124(12) .
K2 K3 4.6807(14) .
K3 O11 2.809(3) .
K3 C38 3.333(5) .
K3 C39 3.348(5) .
K3 Cu1 3.4284(12) 2_766
K3 N5 3.451(5) .
K3 Ge2 3.4926(12) 2_766
K3 Ge4 3.5697(11) 2_766
K3 K3 3.769(2) 2_766
K4 N4 2.820(6) .
K4 N2 2.845(5) .
K4 N3 2.922(6) .
K4 C10 3.311(5) .
C1 C6 1.419(7) .
C1 C2 1.422(6) .
C2 C3 1.400(6) .
C2 C7 1.495(7) .
C3 C4 1.369(7) .
C4 C5 1.379(7) .
C4 C8 1.515(7) .
C5 C6 1.394(7) .
C6 C9 1.505(7) .
C10 C11 1.415(7) .
C10 C15 1.415(6) .
C11 C12 1.394(6) .
C11 C16 1.508(7) .
C12 C13 1.387(8) .
C13 C14 1.371(8) .
C13 C17 1.525(7) .
C14 C15 1.401(7) .
C15 C18 1.499(7) .
C19 O1 1.424(6) .
C19 C20 1.472(8) .
C20 O2 1.430(6) .
C21 O2 1.411(6) .
C21 C22 1.493(8) .
C22 O3 1.420(6) .
C23 O3 1.416(6) .
C23 C24 1.507(8) .
C24 O4 1.413(6) .
C25 O4 1.425(6) .
C25 C26 1.492(7) .
C26 O5 1.421(6) .
C27 O5 1.422(6) .
C27 C28 1.490(7) .
C28 O6 1.417(6) .
C29 O6 1.416(6) .
C29 C30 1.506(7) .
C30 O1 1.419(6) .
C31 O7 1.418(5) .
C31 C32 1.501(7) .
C32 O8 1.424(6) .
C33 O8 1.404(6) .
C33 C34 1.509(8) .
C34 O9 1.422(6) .
C35 O9 1.413(6) .
C35 C36 1.486(7) .
C36 O10 1.398(6) .
C37 O10 1.433(6) .
C37 C38 1.463(7) .
C38 O11 1.425(6) .
C39 O11 1.414(6) .
C39 C40 1.478(7) .
C40 O12 1.423(5) .
C41 O12 1.428(6) .
C41 C42 1.491(7) .
C42 O7 1.415(6) .
N1 K2 3.2124(12) 2_756
