#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:42:22 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178912 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/41/4114187.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_4114187
loop_
_publ_author_name
'Lihung Pu'
'Andrew D. Phillips'
'Anne F. Richards'
'Matthias Stender'
'Richard S. Simons'
'Marilyn M. Olmstead'
'Philip P. Power'
_publ_section_title
;
 Germanium and Tin Analogues of Alkynes and Their Reduction Products
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11626
_journal_page_last               11636
_journal_paper_doi               10.1021/ja035711m
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C75 H105 Ge2 Na'
_chemical_formula_weight         1174.81
_chemical_name_common            '[Bert*Ge]2Na.0.5hexane'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.192(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.2725(15)
_cell_length_b                   20.169(2)
_cell_length_c                   24.160(2)
_cell_measurement_reflns_used    42
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      29.6
_cell_measurement_theta_min      4.3
_cell_volume                     6883.8(12)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens XDISK'
_computing_molecular_graphics    'SHELXTL 5.03, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       2θ-ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Siemens rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9312
_diffrn_reflns_theta_full        56.35
_diffrn_reflns_theta_max         56.35
_diffrn_reflns_theta_min         2.87
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.414
_exptl_absorpt_correction_T_max  0.8054
_exptl_absorpt_correction_T_min  0.5157
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;XABS2: an empirical absorption correction program. Parkin, S.; Moezzi,
 B.; Hope, H. J. Appl. Cryst. 1995, 28, 53-56.
;
_exptl_crystal_colour            'red green dichroic'
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_description       needle
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         8969
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0443P)²+11.5536P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1159
_reflns_number_gt                7064
_reflns_number_total             8969
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja035711msi20030421_060217_3.cif
_cod_data_source_block           mn1090
_cod_original_cell_volume        6884.0(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4114187
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.58556(3) 0.34768(2) 0.227649(19) 0.03610(15) Uani 1 1 d . . .
Ge2 Ge 0.51693(3) 0.27105(2) 0.163302(19) 0.03293(14) Uani 1 1 d . . .
Na1 Na 0.70700(10) 0.32546(7) 0.12963(6) 0.0327(4) Uani 1 1 d . . .
C1 C 0.6729(3) 0.30802(18) 0.29194(15) 0.0257(9) Uani 1 1 d . . .
C2 C 0.7658(3) 0.28579(18) 0.28899(15) 0.0261(9) Uani 1 1 d . . .
C3 C 0.8281(3) 0.2719(2) 0.33720(16) 0.0355(10) Uani 1 1 d . . .
H3 H 0.8905 0.2576 0.3341 0.043 Uiso 1 1 calc R . .
C4 C 0.8012(3) 0.2785(2) 0.38939(17) 0.0391(11) Uani 1 1 d . . .
H4 H 0.8446 0.2692 0.4221 0.047 Uiso 1 1 calc R . .
C5 C 0.7100(3) 0.2988(2) 0.39349(16) 0.0364(10) Uani 1 1 d . . .
H5 H 0.6907 0.3032 0.4293 0.044 Uiso 1 1 calc R . .
C6 C 0.6459(3) 0.31308(18) 0.34587(15) 0.0271(9) Uani 1 1 d . . .
C7 C 0.8029(3) 0.27524(19) 0.23438(15) 0.0267(9) Uani 1 1 d . . .
C8 C 0.7817(3) 0.21595(18) 0.20401(15) 0.0263(9) Uani 1 1 d . . .
C9 C 0.8227(3) 0.2058(2) 0.15583(16) 0.0308(9) Uani 1 1 d . . .
H9 H 0.8077 0.1663 0.1351 0.037 Uiso 1 1 calc R . .
C10 C 0.8846(3) 0.2509(2) 0.13653(16) 0.0316(10) Uani 1 1 d . . .
C11 C 0.9034(3) 0.3089(2) 0.16664(16) 0.0311(10) Uani 1 1 d . . .
H11 H 0.9446 0.3406 0.1539 0.037 Uiso 1 1 calc R . .
C12 C 0.8637(3) 0.32232(19) 0.21522(16) 0.0302(9) Uani 1 1 d . B .
C13 C 0.7193(3) 0.16307(18) 0.22522(16) 0.0320(10) Uani 1 1 d . . .
H13 H 0.6680 0.1863 0.2418 0.038 Uiso 1 1 calc R . .
C14 C 0.7761(3) 0.1216(2) 0.27152(18) 0.0446(12) Uani 1 1 d . . .
H14A H 0.8269 0.0981 0.2563 0.067 Uiso 1 1 calc R . .
H14B H 0.7341 0.0893 0.2858 0.067 Uiso 1 1 calc R . .
H14C H 0.8036 0.1508 0.3020 0.067 Uiso 1 1 calc R . .
C15 C 0.6719(3) 0.1164(2) 0.17958(19) 0.0438(11) Uani 1 1 d . . .
H15A H 0.6393 0.1426 0.1485 0.066 Uiso 1 1 calc R . .
H15B H 0.6260 0.0883 0.1950 0.066 Uiso 1 1 calc R . .
H15C H 0.7201 0.0885 0.1661 0.066 Uiso 1 1 calc R . .
C16 C 0.9306(3) 0.2331(2) 0.08509(18) 0.0456(12) Uani 1 1 d . . .
H16 H 0.8791 0.2178 0.0554 0.055 Uiso 1 1 calc R . .
C17 C 0.9800(6) 0.2865(3) 0.0615(3) 0.141(4) Uani 1 1 d . . .
H17A H 1.0344 0.3003 0.0885 0.212 Uiso 1 1 calc R . .
H17B H 0.9370 0.3242 0.0530 0.212 Uiso 1 1 calc R . .
H17C H 1.0022 0.2712 0.0271 0.212 Uiso 1 1 calc R . .
C18 C 0.9990(5) 0.1768(3) 0.0971(3) 0.103(3) Uani 1 1 d . . .
H18A H 1.0193 0.1616 0.0621 0.155 Uiso 1 1 calc R . .
H18B H 0.9682 0.1401 0.1142 0.155 Uiso 1 1 calc R . .
H18C H 1.0543 0.1917 0.1229 0.155 Uiso 1 1 calc R . .
C19 C 0.8888(3) 0.3866(2) 0.24742(19) 0.0400(11) Uani 1 1 d D . .
H19A H 0.8448 0.3917 0.2759 0.048 Uiso 0.78 1 d P A 1
C20A C 0.8781(5) 0.4478(3) 0.2081(3) 0.0551(17) Uani 0.78 1 d PD B 1
H20A H 0.9160 0.4440 0.1803 0.083 Uiso 0.78 1 d P C 1
H20B H 0.8927 0.4876 0.2319 0.083 Uiso 0.78 1 d P D 1
H20C H 0.8090 0.4510 0.1923 0.083 Uiso 0.78 1 d P E 1
H19B H 0.8630 0.3712 0.2799 0.066 Uiso 0.22 1 d P F 2
C20B C 0.8193(15) 0.4415(10) 0.2355(10) 0.058(6) Uiso 0.22 1 d PD B 2
H20D H 0.8399 0.4790 0.2590 0.087 Uiso 0.22 1 d P G 2
H20E H 0.8096 0.4527 0.1980 0.087 Uiso 0.22 1 d P H 2
H20F H 0.7584 0.4266 0.2470 0.087 Uiso 0.22 1 d P I 2
C21 C 0.9889(4) 0.3869(3) 0.2756(3) 0.091(2) Uani 1 1 d . B .
H21A H 0.9999 0.3482 0.3001 0.136 Uiso 1 1 calc R . .
H21B H 1.0007 0.4275 0.2978 0.136 Uiso 1 1 calc R . .
H21C H 1.0317 0.3854 0.2473 0.136 Uiso 1 1 calc R . .
C22 C 0.5469(3) 0.33046(19) 0.35569(15) 0.0285(9) Uani 1 1 d . . .
C23 C 0.5213(3) 0.39572(19) 0.36529(15) 0.0287(9) Uani 1 1 d . . .
C24 C 0.4350(3) 0.4076(2) 0.38385(16) 0.0330(10) Uani 1 1 d . . .
H24 H 0.4172 0.4521 0.3898 0.040 Uiso 1 1 calc R . .
C25 C 0.3736(3) 0.3567(2) 0.39405(16) 0.0316(10) Uani 1 1 d . . .
C26 C 0.3986(3) 0.29277(19) 0.38178(16) 0.0341(10) Uani 1 1 d . . .
H26 H 0.3562 0.2576 0.3864 0.041 Uiso 1 1 calc R . .
C27 C 0.4840(3) 0.27808(19) 0.36284(16) 0.0327(10) Uani 1 1 d . . .
C28 C 0.5868(3) 0.45373(19) 0.35762(16) 0.0334(10) Uani 1 1 d . . .
H28 H 0.6407 0.4364 0.3396 0.040 Uiso 1 1 calc R . .
C29 C 0.6274(3) 0.4829(2) 0.41421(19) 0.0533(13) Uani 1 1 d . . .
H29A H 0.5758 0.5002 0.4328 0.080 Uiso 1 1 calc R . .
H29B H 0.6712 0.5190 0.4087 0.080 Uiso 1 1 calc R . .
H29C H 0.6614 0.4484 0.4375 0.080 Uiso 1 1 calc R . .
C30 C 0.5362(3) 0.5070(2) 0.31935(19) 0.0469(12) Uani 1 1 d . . .
H30A H 0.5091 0.4869 0.2837 0.070 Uiso 1 1 calc R . .
H30B H 0.5815 0.5415 0.3126 0.070 Uiso 1 1 calc R . .
H30C H 0.4854 0.5268 0.3373 0.070 Uiso 1 1 calc R . .
C31 C 0.2842(3) 0.3699(2) 0.41926(17) 0.0382(10) Uani 1 1 d . . .
H31 H 0.2626 0.3262 0.4325 0.046 Uiso 1 1 calc R . .
C32 C 0.3024(3) 0.4145(2) 0.47025(18) 0.0480(12) Uani 1 1 d . . .
H32A H 0.3524 0.3952 0.4975 0.072 Uiso 1 1 calc R . .
H32B H 0.2442 0.4188 0.4872 0.072 Uiso 1 1 calc R . .
H32C H 0.3223 0.4584 0.4590 0.072 Uiso 1 1 calc R . .
C33 C 0.2047(3) 0.3962(3) 0.37736(19) 0.0614(15) Uani 1 1 d . . .
H33A H 0.1487 0.4037 0.3958 0.092 Uiso 1 1 calc R . .
H33B H 0.1894 0.3639 0.3471 0.092 Uiso 1 1 calc R . .
H33C H 0.2241 0.4381 0.3619 0.092 Uiso 1 1 calc R . .
C34 C 0.5088(3) 0.2063(2) 0.3516(2) 0.0465(12) Uani 1 1 d . . .
H34 H 0.5717 0.2067 0.3379 0.056 Uiso 1 1 calc R . .
C35 C 0.5195(5) 0.1653(3) 0.4038(2) 0.088(2) Uani 1 1 d . . .
H35A H 0.4584 0.1624 0.4177 0.132 Uiso 1 1 calc R . .
H35B H 0.5661 0.1861 0.4323 0.132 Uiso 1 1 calc R . .
H35C H 0.5410 0.1207 0.3956 0.132 Uiso 1 1 calc R . .
C36 C 0.4389(4) 0.1763(2) 0.3058(2) 0.0633(15) Uani 1 1 d . . .
H36A H 0.3770 0.1724 0.3186 0.095 Uiso 1 1 calc R . .
H36B H 0.4609 0.1322 0.2964 0.095 Uiso 1 1 calc R . .
H36C H 0.4333 0.2048 0.2726 0.095 Uiso 1 1 calc R . .
C37 C 0.4243(3) 0.30822(18) 0.10081(15) 0.0240(9) Uani 1 1 d . . .
C38 C 0.3283(3) 0.28864(19) 0.09825(16) 0.0292(9) Uani 1 1 d . . .
C39 C 0.2639(3) 0.2993(2) 0.05078(16) 0.0358(10) Uani 1 1 d . . .
H39 H 0.2004 0.2847 0.0499 0.043 Uiso 1 1 calc R . .
C40 C 0.2902(3) 0.3309(2) 0.00417(16) 0.0356(10) Uani 1 1 d . . .
H40 H 0.2457 0.3372 -0.0286 0.043 Uiso 1 1 calc R . .
C41 C 0.3823(3) 0.35279(19) 0.00664(15) 0.0293(9) Uani 1 1 d . . .
H41 H 0.4006 0.3757 -0.0245 0.035 Uiso 1 1 calc R . .
C42 C 0.4490(3) 0.34208(17) 0.05373(15) 0.0230(8) Uani 1 1 d . . .
C43 C 0.2911(3) 0.25881(19) 0.14773(16) 0.0285(9) Uani 1 1 d . . .
C44 C 0.2597(3) 0.30168(19) 0.18730(16) 0.0275(9) Uani 1 1 d . . .
C45 C 0.2158(3) 0.2744(2) 0.23009(16) 0.0314(9) Uani 1 1 d . . .
H45 H 0.1946 0.3033 0.2568 0.038 Uiso 1 1 calc R . .
C46 C 0.2022(3) 0.2068(2) 0.23501(17) 0.0357(10) Uani 1 1 d . . .
C47 C 0.2357(3) 0.1657(2) 0.19620(19) 0.0400(11) Uani 1 1 d . . .
H47 H 0.2275 0.1191 0.1993 0.048 Uiso 1 1 calc R . .
C48 C 0.2809(3) 0.1898(2) 0.15279(18) 0.0356(10) Uani 1 1 d . . .
C49 C 0.2729(3) 0.37655(19) 0.18361(17) 0.0354(10) Uani 1 1 d . . .
H49 H 0.3233 0.3844 0.1596 0.042 Uiso 1 1 calc R . .
C50 C 0.3060(4) 0.4084(2) 0.24000(18) 0.0504(12) Uani 1 1 d . . .
H50A H 0.2546 0.4072 0.2629 0.076 Uiso 1 1 calc R . .
H50B H 0.3239 0.4546 0.2345 0.076 Uiso 1 1 calc R . .
H50C H 0.3607 0.3841 0.2590 0.076 Uiso 1 1 calc R . .
C51 C 0.1828(4) 0.4097(2) 0.1549(2) 0.0604(14) Uani 1 1 d . . .
H51A H 0.1308 0.4010 0.1763 0.091 Uiso 1 1 calc R . .
H51B H 0.1668 0.3919 0.1170 0.091 Uiso 1 1 calc R . .
H51C H 0.1930 0.4577 0.1529 0.091 Uiso 1 1 calc R . .
C52 C 0.1519(3) 0.1807(2) 0.28208(18) 0.0435(11) Uani 1 1 d . . .
H52 H 0.1699 0.2096 0.3155 0.052 Uiso 1 1 calc R . .
C53 C 0.1779(4) 0.1091(3) 0.2992(3) 0.092(2) Uani 1 1 d . . .
H53A H 0.1551 0.0990 0.3346 0.139 Uiso 1 1 calc R . .
H53B H 0.2468 0.1038 0.3037 0.139 Uiso 1 1 calc R . .
H53C H 0.1484 0.0787 0.2702 0.139 Uiso 1 1 calc R . .
C54 C 0.0457(3) 0.1842(3) 0.2665(2) 0.0518(13) Uani 1 1 d . . .
H54A H 0.0269 0.2299 0.2569 0.078 Uiso 1 1 calc R . .
H54B H 0.0152 0.1695 0.2983 0.078 Uiso 1 1 calc R . .
H54C H 0.0260 0.1553 0.2344 0.078 Uiso 1 1 calc R . .
C55 C 0.3187(3) 0.1418(2) 0.1131(2) 0.0534(13) Uani 1 1 d . . .
H55 H 0.3583 0.1677 0.0898 0.064 Uiso 1 1 calc R . .
C56 C 0.3822(4) 0.0888(3) 0.1447(3) 0.0808(19) Uani 1 1 d . . .
H56A H 0.4339 0.1104 0.1692 0.121 Uiso 1 1 calc R . .
H56B H 0.4085 0.0604 0.1178 0.121 Uiso 1 1 calc R . .
H56C H 0.3448 0.0618 0.1672 0.121 Uiso 1 1 calc R . .
C57 C 0.2379(4) 0.1099(3) 0.0735(2) 0.0741(18) Uani 1 1 d . . .
H57A H 0.1955 0.0864 0.0953 0.111 Uiso 1 1 calc R . .
H57B H 0.2640 0.0785 0.0488 0.111 Uiso 1 1 calc R . .
H57C H 0.2024 0.1445 0.0509 0.111 Uiso 1 1 calc R . .
C58 C 0.5479(3) 0.36667(18) 0.05049(14) 0.0239(9) Uani 1 1 d . . .
C59 C 0.6058(3) 0.33052(18) 0.01876(15) 0.0251(9) Uani 1 1 d . . .
C60 C 0.6943(3) 0.3562(2) 0.01213(16) 0.0322(10) Uani 1 1 d . . .
H60 H 0.7337 0.3314 -0.0087 0.039 Uiso 1 1 calc R . .
C61 C 0.7269(3) 0.4165(2) 0.03486(16) 0.0328(10) Uani 1 1 d . K .
C62 C 0.6691(3) 0.45072(19) 0.06688(16) 0.0311(10) Uani 1 1 d . . .
H62 H 0.6910 0.4915 0.0837 0.037 Uiso 1 1 calc R . .
C63 C 0.5800(3) 0.42725(18) 0.07526(15) 0.0261(9) Uani 1 1 d . . .
C64 C 0.5748(3) 0.2644(2) -0.00790(16) 0.0346(10) Uani 1 1 d . . .
H64 H 0.5091 0.2554 0.0000 0.041 Uiso 1 1 calc R . .
C65 C 0.5716(3) 0.2663(2) -0.07134(17) 0.0501(12) Uani 1 1 d . . .
H65A H 0.5282 0.3013 -0.0871 0.075 Uiso 1 1 calc R . .
H65B H 0.5495 0.2234 -0.0872 0.075 Uiso 1 1 calc R . .
H65C H 0.6352 0.2753 -0.0804 0.075 Uiso 1 1 calc R . .
C66 C 0.6384(3) 0.2082(2) 0.01854(18) 0.0454(12) Uani 1 1 d . . .
H66A H 0.7041 0.2171 0.0134 0.068 Uiso 1 1 calc R . .
H66B H 0.6179 0.1661 0.0005 0.068 Uiso 1 1 calc R . .
H66C H 0.6339 0.2055 0.0586 0.068 Uiso 1 1 calc R . .
C67 C 0.8220(3) 0.4431(2) 0.0222(2) 0.0534(13) Uani 1 1 d D . .
C68 C 0.8191(5) 0.4604(5) -0.0371(3) 0.132(3) Uani 1 1 d . K .
H68A H 0.7793 0.4954 -0.0474 0.197 Uiso 1 1 d . . .
H68B H 0.7991 0.4208 -0.0598 0.197 Uiso 1 1 d . . .
H68C H 0.8838 0.4699 -0.0437 0.197 Uiso 1 1 d . . .
H67A H 0.8671 0.4066 0.0303 0.158 Uiso 0.50 1 d P J 1
C69A C 0.8431(11) 0.5118(6) 0.0481(6) 0.083(5) Uani 0.50 1 d PD K 1
H69A H 0.9026 0.5266 0.0372 0.124 Uiso 0.50 1 d P L 1
H69B H 0.7938 0.5416 0.0307 0.124 Uiso 0.50 1 d P M 1
H69C H 0.8451 0.5098 0.0861 0.124 Uiso 0.50 1 d P N 1
H67B H 0.8579 0.4024 0.0238 0.099 Uiso 0.50 1 d P O 2
C69B C 0.8813(9) 0.4778(8) 0.0668(6) 0.075(4) Uani 0.50 1 d PD K 2
H69D H 0.9339 0.4931 0.0515 0.113 Uiso 0.50 1 d P P 2
H69E H 0.8411 0.5173 0.0730 0.113 Uiso 0.50 1 d P Q 2
H69F H 0.8908 0.4519 0.0967 0.113 Uiso 0.50 1 d P R 2
C70 C 0.5173(3) 0.46759(19) 0.10868(15) 0.0292(9) Uani 1 1 d . . .
H70 H 0.4823 0.4356 0.1298 0.035 Uiso 1 1 calc R . .
C71 C 0.5723(3) 0.5144(2) 0.15144(17) 0.0424(11) Uani 1 1 d . . .
H71A H 0.6224 0.4896 0.1746 0.064 Uiso 1 1 calc R . .
H71B H 0.5292 0.5335 0.1753 0.064 Uiso 1 1 calc R . .
H71C H 0.6006 0.5501 0.1318 0.064 Uiso 1 1 calc R . .
C72 C 0.4438(3) 0.5068(2) 0.06976(17) 0.0400(11) Uani 1 1 d . . .
H72A H 0.4759 0.5396 0.0492 0.060 Uiso 1 1 calc R . .
H72B H 0.4010 0.5294 0.0918 0.060 Uiso 1 1 calc R . .
H72C H 0.4074 0.4764 0.0432 0.060 Uiso 1 1 calc R . .
C73 C 0.4926(7) -0.0313(4) 0.0106(4) 0.049(2) Uiso 0.50 1 d P . 1
H73A H 0.4653 -0.0585 -0.0218 0.059 Uiso 0.50 1 calc PR . 1
H73C H 0.4419 -0.0259 0.0342 0.059 Uiso 0.50 1 calc PR . 1
C74 C 0.5639(7) -0.0718(5) 0.0423(4) 0.050(2) Uiso 0.50 1 d P S 1
H74A H 0.5357 -0.1151 0.0501 0.059 Uiso 0.50 1 calc PR S 1
H74B H 0.6153 -0.0803 0.0197 0.059 Uiso 0.50 1 calc PR S 1
C75 C 0.6016(9) -0.0430(6) 0.0920(5) 0.085(4) Uiso 0.50 1 d P S 1
H75A H 0.6511 -0.0717 0.1114 0.127 Uiso 0.50 1 calc PR S 1
H75B H 0.5517 -0.0368 0.1155 0.127 Uiso 0.50 1 calc PR S 1
H75C H 0.6290 0.0001 0.0846 0.127 Uiso 0.50 1 calc PR S 1
C76 C 0.4154 0.0053 -0.0667 0.050 Uiso 0.25 1 d P . 2
H76A H 0.4006 0.0504 -0.0587 0.075 Uiso 0.25 1 d P T 2
H76B H 0.4360 0.0030 -0.1028 0.075 Uiso 0.25 1 d P U 2
H76C H 0.3601 -0.0217 -0.0666 0.075 Uiso 0.25 1 d P V 2
C77 C 0.4862 -0.0172 -0.0267 0.050 Uiso 0.25 1 d P . 2
H77A H 0.4637 -0.0112 0.0086 0.060 Uiso 0.25 1 d P W 2
H77B H 0.5381 0.0130 -0.0269 0.060 Uiso 0.25 1 d P X 2
C78 C 0.5250 -0.0806 -0.0254 0.050 Uiso 0.25 1 d P Y 2
H78A H 0.5572 -0.0839 -0.0576 0.060 Uiso 0.25 1 d P Z 2
H78B H 0.4725 -0.1108 -0.0316 0.060 Uiso 0.25 1 d P A 2
C79 C 0.5829 -0.1046 0.0165 0.050 Uiso 0.25 1 d P Y 2
H79A H 0.6390 -0.1172 0.0014 0.060 Uiso 0.25 1 d P B 2
H79B H 0.5545 -0.1451 0.0268 0.060 Uiso 0.25 1 d P C 2
C80 C 0.6156 -0.0706 0.0686 0.050 Uiso 0.25 1 d P . 2
H80A H 0.6515 -0.0380 0.0517 0.060 Uiso 0.25 1 d P D 2
H80B H 0.6621 -0.1035 0.0817 0.060 Uiso 0.25 1 d P E 2
C81 C 0.6213 -0.0417 0.1138 0.050 Uiso 0.25 1 d P . 2
H81A H 0.6864 -0.0316 0.1270 0.075 Uiso 0.25 1 d P F 2
H81B H 0.5854 -0.0013 0.1092 0.075 Uiso 0.25 1 d P G 2
H81C H 0.5965 -0.0696 0.1405 0.075 Uiso 0.25 1 d P H 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C1 Ge1 Ge2 114.21(10) . .
C1 Ge1 Na1 100.15(11) . .
Ge2 Ge1 Na1 68.02(3) . .
C37 Ge2 Ge1 115.32(10) . .
C37 Ge2 Na1 100.11(11) . .
Ge1 Ge2 Na1 68.97(3) . .
C12 Na1 C11 28.65(11) . .
C12 Na1 C59 158.36(12) . .
C11 Na1 C59 130.11(12) . .
C12 Na1 C58 164.19(12) . .
C11 Na1 C58 153.46(12) . .
C59 Na1 C58 28.42(10) . .
C12 Na1 C7 28.55(11) . .
C11 Na1 C7 50.06(11) . .
C59 Na1 C7 161.49(12) . .
C58 Na1 C7 156.40(12) . .
C12 Na1 C60 131.13(12) . .
C11 Na1 C60 104.84(12) . .
C59 Na1 C60 28.12(11) . .
C58 Na1 C60 49.51(11) . .
C7 Na1 C60 153.39(12) . .
C12 Na1 C63 136.12(12) . .
C11 Na1 C63 138.21(12) . .
C59 Na1 C63 49.88(10) . .
C58 Na1 C63 28.10(10) . .
C7 Na1 C63 145.83(12) . .
C60 Na1 C63 57.25(11) . .
C12 Na1 C10 50.08(11) . .
C11 Na1 C10 27.68(11) . .
C59 Na1 C10 112.91(12) . .
C58 Na1 C10 141.32(12) . .
C7 Na1 C10 58.09(11) . .
C60 Na1 C10 95.67(12) . .
C63 Na1 C10 149.48(12) . .
C12 Na1 C9 57.45(11) . .
C11 Na1 C9 48.44(12) . .
C59 Na1 C9 115.11(12) . .
C58 Na1 C9 138.26(12) . .
C7 Na1 C9 48.80(11) . .
C60 Na1 C9 110.04(12) . .
C63 Na1 C9 164.98(12) . .
C10 Na1 C9 27.46(11) . .
C12 Na1 C8 49.96(11) . .
C11 Na1 C8 57.62(11) . .
C59 Na1 C8 133.50(12) . .
C58 Na1 C8 143.57(12) . .
C7 Na1 C8 28.01(10) . .
C60 Na1 C8 136.62(12) . .
C63 Na1 C8 161.25(12) . .
C10 Na1 C8 49.19(11) . .
C9 Na1 C8 27.29(10) . .
C12 Na1 C62 117.57(12) . .
C11 Na1 C62 111.26(12) . .
C59 Na1 C62 57.17(11) . .
C58 Na1 C62 48.89(11) . .
C7 Na1 C62 141.20(12) . .
C60 Na1 C62 47.99(11) . .
C63 Na1 C62 27.50(10) . .
C10 Na1 C62 124.13(12) . .
C9 Na1 C62 150.17(12) . .
C8 Na1 C62 167.48(12) . .
C12 Na1 C61 115.11(12) . .
C11 Na1 C61 96.70(11) . .
C59 Na1 C61 49.38(11) . .
C58 Na1 C61 57.56(10) . .
C7 Na1 C61 143.64(12) . .
C60 Na1 C61 27.31(11) . .
C63 Na1 C61 48.91(11) . .
C10 Na1 C61 100.58(11) . .
C9 Na1 C61 123.99(12) . .
C8 Na1 C61 149.74(12) . .
C62 Na1 C61 27.11(11) . .
C2 C1 C6 116.8(3) . .
C2 C1 Ge1 124.8(3) . .
C6 C1 Ge1 117.5(3) . .
C3 C2 C1 121.0(3) . .
C3 C2 C7 116.3(3) . .
C1 C2 C7 122.7(3) . .
C4 C3 C2 121.4(4) . .
C3 C4 C5 118.9(4) . .
C4 C5 C6 121.1(4) . .
C5 C6 C1 120.8(4) . .
C5 C6 C22 116.0(3) . .
C1 C6 C22 123.1(3) . .
C12 C7 C8 119.8(3) . .
C12 C7 C2 120.2(3) . .
C8 C7 C2 119.9(3) . .
C12 C7 Na1 73.3(2) . .
C8 C7 Na1 78.6(2) . .
C2 C7 Na1 122.5(2) . .
C9 C8 C7 118.4(3) . .
C9 C8 C13 120.9(3) . .
C7 C8 C13 120.6(3) . .
C9 C8 Na1 76.0(2) . .
C7 C8 Na1 73.4(2) . .
C13 C8 Na1 123.4(2) . .
C8 C9 C10 123.1(4) . .
C8 C9 Na1 76.7(2) . .
C10 C9 Na1 75.9(2) . .
C11 C10 C9 117.4(4) . .
C11 C10 C16 123.5(4) . .
C9 C10 C16 119.0(4) . .
C11 C10 Na1 72.4(2) . .
C9 C10 Na1 76.7(2) . .
C16 C10 Na1 122.8(3) . .
C10 C11 C12 122.2(4) . .
C10 C11 Na1 79.9(2) . .
C12 C11 Na1 75.0(2) . .
C11 C12 C7 119.1(4) . .
C11 C12 C19 119.8(4) . .
C7 C12 C19 121.0(4) . .
C11 C12 Na1 76.3(2) . .
C7 C12 Na1 78.2(2) . .
C19 C12 Na1 117.3(2) . .
C8 C13 C15 114.0(3) . .
C8 C13 C14 110.7(3) . .
C15 C13 C14 108.9(3) . .
C17 C16 C18 107.5(5) . .
C17 C16 C10 115.8(4) . .
C18 C16 C10 111.3(4) . .
C20B C19 C21 130.8(10) . .
C20B C19 C12 115.6(10) . .
C21 C19 C12 112.1(4) . .
C21 C19 C20A 106.2(4) . .
C12 C19 C20A 111.6(4) . .
C23 C22 C27 119.9(4) . .
C23 C22 C6 121.3(3) . .
C27 C22 C6 118.1(3) . .
C24 C23 C22 118.8(4) . .
C24 C23 C28 119.6(3) . .
C22 C23 C28 121.6(3) . .
C23 C24 C25 122.6(4) . .
C26 C25 C24 117.4(4) . .
C26 C25 C31 120.6(4) . .
C24 C25 C31 122.0(4) . .
C25 C26 C27 122.3(4) . .
C26 C27 C22 118.8(4) . .
C26 C27 C34 119.8(4) . .
C22 C27 C34 121.4(4) . .
C29 C28 C23 110.4(3) . .
C29 C28 C30 110.9(4) . .
C23 C28 C30 111.5(3) . .
C33 C31 C25 112.9(3) . .
C33 C31 C32 111.2(4) . .
C25 C31 C32 112.0(3) . .
C35 C34 C36 112.0(4) . .
C35 C34 C27 111.8(4) . .
C36 C34 C27 111.5(4) . .
C42 C37 C38 116.7(3) . .
C42 C37 Ge2 125.0(3) . .
C38 C37 Ge2 117.2(3) . .
C39 C38 C37 121.2(4) . .
C39 C38 C43 117.1(3) . .
C37 C38 C43 121.7(3) . .
C38 C39 C40 121.3(4) . .
C41 C40 C39 118.5(4) . .
C40 C41 C42 121.4(4) . .
C41 C42 C37 120.9(3) . .
C41 C42 C58 116.3(3) . .
C37 C42 C58 122.9(3) . .
C48 C43 C44 120.1(4) . .
C48 C43 C38 121.2(3) . .
C44 C43 C38 118.5(3) . .
C45 C44 C43 118.7(4) . .
C45 C44 C49 120.3(3) . .
C43 C44 C49 120.9(3) . .
C46 C45 C44 122.4(4) . .
C45 C46 C47 117.7(4) . .
C45 C46 C52 119.4(4) . .
C47 C46 C52 122.9(4) . .
C46 C47 C48 122.7(4) . .
C47 C48 C43 118.4(4) . .
C47 C48 C55 119.7(4) . .
C43 C48 C55 121.8(4) . .
C50 C49 C51 110.9(4) . .
C50 C49 C44 113.0(3) . .
C51 C49 C44 111.0(4) . .
C54 C52 C46 111.2(4) . .
C54 C52 C53 107.8(4) . .
C46 C52 C53 113.9(4) . .
C48 C55 C56 111.7(4) . .
C48 C55 C57 111.1(4) . .
C56 C55 C57 111.0(4) . .
C59 C58 C63 120.0(3) . .
C59 C58 C42 118.9(3) . .
C63 C58 C42 120.9(3) . .
C59 C58 Na1 75.1(2) . .
C63 C58 Na1 77.9(2) . .
C42 C58 Na1 121.8(2) . .
C60 C59 C58 118.8(3) . .
C60 C59 C64 119.4(3) . .
C58 C59 C64 121.9(3) . .
C60 C59 Na1 77.0(2) . .
C58 C59 Na1 76.4(2) . .
C64 C59 Na1 116.3(2) . .
C61 C60 C59 122.6(4) . .
C61 C60 Na1 80.1(2) . .
C59 C60 Na1 74.8(2) . .
C60 C61 C62 117.5(4) . .
C60 C61 C67 119.0(4) . .
C62 C61 C67 123.5(4) . .
C60 C61 Na1 72.5(2) . .
C62 C61 Na1 75.5(2) . .
C67 C61 Na1 123.6(3) . .
C61 C62 C63 122.4(4) . .
C61 C62 Na1 77.4(2) . .
C63 C62 Na1 74.9(2) . .
C62 C63 C58 118.7(3) . .
C62 C63 C70 120.7(3) . .
C58 C63 C70 120.5(3) . .
C62 C63 Na1 77.6(2) . .
C58 C63 Na1 74.0(2) . .
C70 C63 Na1 120.7(2) . .
C59 C64 C65 111.6(3) . .
C59 C64 C66 110.7(3) . .
C65 C64 C66 111.5(3) . .
C69B C67 C68 122.8(8) . .
C69B C67 C61 117.4(7) . .
C68 C67 C61 112.1(4) . .
C68 C67 C69A 99.2(8) . .
C61 C67 C69A 111.2(6) . .
C63 C70 C72 110.7(3) . .
C63 C70 C71 113.7(3) . .
C72 C70 C71 109.8(3) . .
C73 C73 C74 125.4(11) 3_655 .
C75 C74 C73 112.6(9) . .
C77 C76 C80 122.4 . 3_655
C76 C77 C78 124.8 . .
C76 C77 C77 122.8 . 3_655
C78 C77 C77 111.0 . 3_655
C79 C78 C77 124.3 . .
C78 C79 C80 126.0 . .
C76 C80 C79 111.0 3_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ge1 C1 2.014(4) .
Ge1 Ge2 2.3089(7) .
Ge1 Na1 3.1596(15) .
Ge2 C37 2.005(4) .
Ge2 Na1 3.1391(15) .
Na1 C12 2.822(4) .
Na1 C11 2.838(4) .
Na1 C59 2.858(4) .
Na1 C58 2.875(4) .
Na1 C7 2.884(4) .
Na1 C60 2.886(4) .
Na1 C63 2.923(4) .
Na1 C10 2.931(4) .
Na1 C9 2.941(4) .
Na1 C8 2.950(4) .
Na1 C62 2.956(4) .
Na1 C61 2.981(4) .
C1 C2 1.411(5) .
C1 C6 1.414(5) .
C2 C3 1.389(5) .
C2 C7 1.505(5) .
C3 C4 1.376(6) .
C4 C5 1.382(6) .
C5 C6 1.394(5) .
C6 C22 1.507(5) .
C7 C12 1.408(5) .
C7 C8 1.413(5) .
C8 C9 1.390(5) .
C8 C13 1.525(5) .
C9 C10 1.394(5) .
C10 C11 1.383(6) .
C10 C16 1.529(5) .
C11 C12 1.401(5) .
C12 C19 1.528(6) .
C13 C15 1.531(6) .
C13 C14 1.533(5) .
C16 C17 1.448(7) .
C16 C18 1.499(7) .
C19 C20B 1.488(14) .
C19 C21 1.491(6) .
C19 C20A 1.551(7) .
C22 C23 1.394(5) .
C22 C27 1.413(5) .
C23 C24 1.390(5) .
C23 C28 1.526(5) .
C24 C25 1.394(5) .
C25 C26 1.381(5) .
C25 C31 1.514(5) .
C26 C27 1.393(5) .
C27 C34 1.523(5) .
C28 C29 1.525(6) .
C28 C30 1.531(6) .
C31 C33 1.506(6) .
C31 C32 1.519(6) .
C34 C35 1.499(7) .
C34 C36 1.507(6) .
C37 C42 1.413(5) .
C37 C38 1.419(5) .
C38 C39 1.381(5) .
C38 C43 1.501(5) .
C39 C40 1.391(6) .
C40 C41 1.380(5) .
C41 C42 1.392(5) .
C42 C58 1.510(5) .
C43 C48 1.406(5) .
C43 C44 1.409(5) .
C44 C45 1.396(5) .
C44 C49 1.526(5) .
C45 C46 1.386(6) .
C46 C47 1.387(6) .
C46 C52 1.522(6) .
C47 C48 1.396(6) .
C48 C55 1.515(6) .
C49 C50 1.519(6) .
C49 C51 1.525(6) .
C52 C54 1.511(6) .
C52 C53 1.534(7) .
C55 C56 1.531(7) .
C55 C57 1.532(7) .
C58 C59 1.407(5) .
C58 C63 1.408(5) .
C59 C60 1.396(5) .
C59 C64 1.519(5) .
C60 C61 1.388(6) .
C61 C62 1.391(5) .
C61 C67 1.529(6) .
C62 C63 1.398(5) .
C63 C70 1.524(5) .
C64 C65 1.527(5) .
C64 C66 1.534(6) .
C67 C69B 1.453(11) .
C67 C68 1.468(8) .
C67 C69A 1.533(12) .
C70 C72 1.525(5) .
C70 C71 1.532(5) .
C73 C73 1.390(17) 3_655
C73 C74 1.438(12) .
C74 C75 1.373(14) .
C76 C77 1.3721 .
C76 C80 1.3881 3_655
C76 C81 1.3923 3_655
C77 C78 1.3921 .
C77 C77 1.4684 3_655
C78 C79 1.3052 .
C79 C80 1.4509 .
C80 C81 1.2303 .
C80 C76 1.3881 3_655
C81 C76 1.3923 3_655
