# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_jwang378 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[[{Mn(C6N4H18)(C6N4H20)}{Mn(C6N4H18)}4V15Ge6O48(0.5H2O)]*(C6N4H18)*2H2O' _chemical_melting_point ? _chemical_formula_moiety C42H133N28Mn5V15Ge6O50.5 _chemical_formula_sum 'C36 H115 Ge6 Mn5 N24 O50.50 V15' _chemical_formula_weight 3313.03 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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 14.9927(4) _cell_length_b 24.6112(5) _cell_length_c 30.6670(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11315.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 19076 _cell_measurement_theta_min 1.51 _cell_measurement_theta_max 24.76 _exptl_crystal_description rhombus _exptl_crystal_colour black _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.95 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6260 _exptl_absorpt_coefficient_mu 3.357 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.5192 _exptl_absorpt_correction_T_max 0.7192 _exptl_absorpt_process_details 'X-Shape (STOE & CIE, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Imaging Plate Diffraction System' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 92172 _diffrn_reflns_av_R_equivalents 0.0986 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 24.76 _reflns_number_total 19076 _reflns_number_gt 16246 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE-IPDS Program Package' _computing_cell_refinement 'STOE-IPDS Program Package' _computing_data_reduction 'STOE-IPDS Program Package' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+40.9234P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 19076 _refine_ls_number_parameters 1177 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0794 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.1493 _refine_ls_wR_factor_gt 0.1427 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.000 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1 Ge 0.52181(8) 0.42207(5) 0.33955(4) 0.0481(3) Uani 1 1 d . . . Ge2 Ge 0.85099(8) 0.63960(4) 0.24433(4) 0.0449(3) Uani 1 1 d . . . Ge3 Ge 0.77059(8) 0.28018(4) 0.20817(4) 0.0452(3) Uani 1 1 d . . . Ge4 Ge 0.95738(8) 0.32571(4) 0.22164(4) 0.0453(3) Uani 1 1 d . . . Ge5 Ge 0.91450(8) 0.58037(5) 0.16385(4) 0.0460(3) Uani 1 1 d . . . Ge6 Ge 0.47121(8) 0.52072(5) 0.28827(4) 0.0459(3) Uani 1 1 d . . . V1 V 0.95694(13) 0.42157(8) 0.30184(6) 0.0474(4) Uani 1 1 d . . . V2 V 0.64438(13) 0.60271(7) 0.27167(6) 0.0457(4) Uani 1 1 d . . . V3 V 0.74126(13) 0.41815(7) 0.36049(6) 0.0444(4) Uani 1 1 d . . . V4 V 0.50402(13) 0.40200(7) 0.22917(6) 0.0462(4) Uani 1 1 d . . . V5 V 0.76171(13) 0.49217(7) 0.12652(6) 0.0429(4) Uani 1 1 d . . . V6 V 0.62491(13) 0.32653(7) 0.28063(7) 0.0459(4) Uani 1 1 d . . . V7 V 0.84555(13) 0.55110(7) 0.33052(6) 0.0469(4) Uani 1 1 d . . . V8 V 0.81772(13) 0.33129(7) 0.31055(6) 0.0455(4) Uani 1 1 d . . . V9 V 0.98656(13) 0.52641(7) 0.26086(7) 0.0476(5) Uani 1 1 d . . . V10 V 0.97622(13) 0.45133(7) 0.18247(7) 0.0466(4) Uani 1 1 d . . . V11 V 0.66179(14) 0.53198(7) 0.35161(6) 0.0469(4) Uani 1 1 d . . . V12 V 0.63268(13) 0.37243(7) 0.16376(6) 0.0447(4) Uani 1 1 d . . . V13 V 0.82991(13) 0.38547(7) 0.13961(6) 0.0450(4) Uani 1 1 d . . . V14 V 0.54802(13) 0.51057(7) 0.18609(6) 0.0434(4) Uani 1 1 d . . . V15 V 0.68623(13) 0.59028(7) 0.17528(6) 0.0441(4) Uani 1 1 d . . . O1 O 0.7298(5) 0.5807(3) 0.3147(2) 0.0507(18) Uani 1 1 d . . . O2 O 1.0862(6) 0.5480(4) 0.2725(3) 0.066(2) Uani 1 1 d . . . O3 O 0.9755(6) 0.5924(4) 0.1173(3) 0.070(2) Uani 1 1 d . . . O4 O 1.0676(6) 0.4457(3) 0.1567(3) 0.067(2) Uani 1 1 d . . . O5 O 0.5716(5) 0.5496(3) 0.3059(2) 0.0489(18) Uani 1 1 d . . . O6 O 0.7456(5) 0.4010(3) 0.4097(2) 0.0519(19) Uani 1 1 d . . . O7 O 0.9250(5) 0.3494(3) 0.2729(3) 0.0524(19) Uani 1 1 d . . . O8 O 1.0432(5) 0.4097(3) 0.3315(3) 0.063(2) Uani 1 1 d . . . O9 O 0.8872(5) 0.5850(3) 0.3697(3) 0.055(2) Uani 1 1 d . . . O10 O 0.4825(6) 0.3830(4) 0.3819(3) 0.067(2) Uani 1 1 d . . . O11 O 0.3876(6) 0.5656(3) 0.2809(3) 0.066(2) Uani 1 1 d . . . O12 O 0.9917(5) 0.4503(3) 0.2446(3) 0.0514(19) Uani 1 1 d . . . O13 O 0.9642(5) 0.5304(3) 0.1972(3) 0.0513(19) Uani 1 1 d . . . O14 O 0.6357(6) 0.5587(3) 0.3968(3) 0.060(2) Uani 1 1 d . . . O15 O 0.8984(5) 0.5874(3) 0.2756(3) 0.053(2) Uani 1 1 d . . . O16 O 0.8485(6) 0.2816(3) 0.3417(3) 0.063(2) Uani 1 1 d . . . O17 O 0.4630(5) 0.5306(3) 0.1596(3) 0.055(2) Uani 1 1 d . . . O18 O 0.8042(5) 0.5616(3) 0.1536(2) 0.0485(18) Uani 1 1 d . . . O19 O 0.7193(5) 0.2211(3) 0.1942(3) 0.055(2) Uani 1 1 d . . . O20 O 0.8874(5) 0.2703(3) 0.2092(3) 0.0486(18) Uani 1 1 d . . . O21 O 0.6041(6) 0.6615(3) 0.2832(3) 0.060(2) Uani 1 1 d . . . O22 O 0.6226(5) 0.4549(3) 0.3515(3) 0.0514(19) Uani 1 1 d . . . O23 O 0.5781(6) 0.2715(3) 0.2962(3) 0.062(2) Uani 1 1 d . . . O24 O 0.5829(6) 0.3396(3) 0.1264(3) 0.057(2) Uani 1 1 d . . . O25 O 0.8552(6) 0.3583(4) 0.0944(3) 0.062(2) Uani 1 1 d . . . O26 O 0.6997(5) 0.3574(3) 0.3255(2) 0.0511(19) Uani 1 1 d . . . O27 O 0.7456(5) 0.3040(3) 0.2605(3) 0.0496(19) Uani 1 1 d . . . O28 O 0.5958(5) 0.5724(3) 0.2182(3) 0.0471(18) Uani 1 1 d . . . O29 O 0.4439(5) 0.4727(3) 0.3297(2) 0.0466(18) Uani 1 1 d . . . O30 O 0.8738(5) 0.4587(3) 0.1435(2) 0.0453(17) Uani 1 1 d . . . O31 O 0.9104(5) 0.6400(3) 0.1949(3) 0.0461(18) Uani 1 1 d . . . O32 O 0.7613(5) 0.5004(3) 0.0747(2) 0.0487(18) Uani 1 1 d . . . O33 O 0.4064(5) 0.3785(3) 0.2171(3) 0.058(2) Uani 1 1 d . . . O34 O 0.7722(5) 0.4946(3) 0.3564(2) 0.0502(18) Uani 1 1 d . . . O35 O 0.8535(5) 0.4002(3) 0.3338(2) 0.0486(18) Uani 1 1 d . . . O36 O 0.5942(5) 0.3465(3) 0.2208(2) 0.0525(19) Uani 1 1 d . . . O37 O 0.8496(5) 0.7040(3) 0.2650(3) 0.0504(19) Uani 1 1 d . . . O38 O 0.4968(5) 0.4818(3) 0.2422(2) 0.0500(18) Uani 1 1 d . . . O39 O 0.5588(5) 0.4325(3) 0.1786(2) 0.0487(18) Uani 1 1 d . . . O40 O 0.9281(5) 0.4975(3) 0.3101(3) 0.0506(19) Uani 1 1 d . . . O41 O 0.7517(5) 0.3348(3) 0.1723(2) 0.0475(18) Uani 1 1 d . . . O42 O 1.0653(5) 0.3041(3) 0.2182(3) 0.0483(18) Uani 1 1 d . . . O43 O 0.6558(6) 0.6383(3) 0.1439(3) 0.059(2) Uani 1 1 d . . . O44 O 0.6540(5) 0.5210(3) 0.1504(2) 0.0500(18) Uani 1 1 d . . . O45 O 0.9301(5) 0.3756(3) 0.1836(2) 0.0481(18) Uani 1 1 d . . . O46 O 0.7164(5) 0.4214(3) 0.1353(2) 0.0454(17) Uani 1 1 d . . . O47 O 0.7444(5) 0.6170(3) 0.2299(2) 0.0474(18) Uani 1 1 d . . . O48 O 0.5339(5) 0.3846(3) 0.2917(2) 0.0494(18) Uani 1 1 d . . . Mn1 Mn 1.11480(14) 0.23974(7) 0.17494(6) 0.0563(5) Uani 1 1 d . . . Mn2 Mn 1.16480(12) 0.28815(7) 0.26664(6) 0.0514(4) Uani 1 1 d . . . Mn3 Mn 0.32857(14) 0.59310(8) 0.22579(8) 0.0669(6) Uani 1 1 d . . . Mn4 Mn 0.63944(18) 0.20788(11) 0.14339(8) 0.0848(7) Uani 1 1 d . . . Mn5 Mn 0.68826(18) 0.51708(10) 0.01169(7) 0.0780(6) Uani 1 1 d . . . N11 N 1.0703(9) 0.2571(5) 0.1040(4) 0.077(3) Uani 1 1 d . . . N12 N 1.2148(8) 0.1913(5) 0.1367(4) 0.072(3) Uiso 1 1 d . . . H1N H 1.2690 0.1938 0.1492 0.086 Uiso 1 1 calc R . . H2N H 1.1988 0.1560 0.1362 0.086 Uiso 1 1 calc R . . N13 N 1.1937(11) 0.3250(5) 0.1510(5) 0.094(4) Uani 1 1 d . . . H3N H 1.1814 0.3521 0.1697 0.113 Uiso 1 1 calc R . . H4N H 1.2530 0.3194 0.1512 0.113 Uiso 1 1 calc R . . N14 N 0.9941(7) 0.1859(4) 0.1687(4) 0.068(3) Uani 1 1 d . . . H5N H 1.0084 0.1518 0.1767 0.081 Uiso 1 1 calc R . . H6N H 0.9508 0.1979 0.1866 0.081 Uiso 1 1 calc R . . C11 C 1.1253(16) 0.2235(12) 0.0731(7) 0.151(11) Uani 1 1 d . . . H11A H 1.0963 0.1887 0.0687 0.181 Uiso 1 1 calc R . . H11B H 1.1284 0.2418 0.0451 0.181 Uiso 1 1 calc R . . C12 C 1.2180(11) 0.2142(6) 0.0899(5) 0.080(4) Uani 1 1 d . . . H12A H 1.2508 0.2482 0.0897 0.096 Uiso 1 1 calc R . . H12B H 1.2489 0.1888 0.0710 0.096 Uiso 1 1 calc R . . C13 C 1.0796(15) 0.3179(8) 0.0970(7) 0.111(7) Uani 1 1 d . . . H13A H 1.0645 0.3258 0.0669 0.134 Uiso 1 1 calc R . . H13B H 1.0359 0.3360 0.1153 0.134 Uiso 1 1 calc R . . C14 C 1.1643(14) 0.3408(8) 0.1059(6) 0.103(6) Uani 1 1 d . . . H14A H 1.1610 0.3801 0.1037 0.123 Uiso 1 1 calc R . . H14B H 1.2074 0.3280 0.0847 0.123 Uiso 1 1 calc R . . C15 C 0.9715(13) 0.2383(8) 0.1012(5) 0.101(6) Uani 1 1 d . . . H15A H 0.9335 0.2649 0.1154 0.121 Uiso 1 1 calc R . . H15B H 0.9537 0.2359 0.0708 0.121 Uiso 1 1 calc R . . C16 C 0.9601(12) 0.1857(7) 0.1220(6) 0.091(5) Uani 1 1 d . . . H16A H 0.9921 0.1584 0.1054 0.109 Uiso 1 1 calc R . . H16B H 0.8974 0.1761 0.1219 0.109 Uiso 1 1 calc R . . N21 N 1.2498(8) 0.3033(5) 0.3306(4) 0.072(3) Uani 1 1 d . . . N22 N 1.3090(7) 0.2732(4) 0.2462(4) 0.060(3) Uani 1 1 d . . . H7N H 1.3115 0.2499 0.2237 0.072 Uiso 1 1 calc R . . H8N H 1.3355 0.3045 0.2384 0.072 Uiso 1 1 calc R . . N23 N 1.1944(8) 0.3811(4) 0.2669(4) 0.070(3) Uani 1 1 d . . . H9N H 1.2181 0.3907 0.2411 0.085 Uiso 1 1 calc R . . H10N H 1.1429 0.3995 0.2703 0.085 Uiso 1 1 calc R . . N24 N 1.0714(7) 0.2635(4) 0.3199(3) 0.062(3) Uani 1 1 d . . . H11N H 1.0195 0.2814 0.3167 0.075 Uiso 1 1 calc R . . H12N H 1.0600 0.2277 0.3176 0.075 Uiso 1 1 calc R . . C21 C 1.3454(10) 0.2879(7) 0.3239(5) 0.089(5) Uani 1 1 d . . . H21A H 1.3682 0.2707 0.3501 0.106 Uiso 1 1 calc R . . H21B H 1.3805 0.3202 0.3183 0.106 Uiso 1 1 calc R . . C22 C 1.3537(10) 0.2493(5) 0.2861(6) 0.083(5) Uani 1 1 d . . . H22A H 1.3259 0.2149 0.2934 0.100 Uiso 1 1 calc R . . H22B H 1.4162 0.2426 0.2799 0.100 Uiso 1 1 calc R . . C23 C 1.2466(9) 0.3629(6) 0.3397(5) 0.078(4) Uani 1 1 d . . . H23A H 1.1906 0.3715 0.3540 0.093 Uiso 1 1 calc R . . H23B H 1.2944 0.3721 0.3597 0.093 Uiso 1 1 calc R . . C24 C 1.2550(9) 0.3958(5) 0.3014(5) 0.071(4) Uani 1 1 d . . . H24A H 1.3156 0.3929 0.2906 0.086 Uiso 1 1 calc R . . H24B H 1.2447 0.4334 0.3093 0.086 Uiso 1 1 calc R . . C25 C 1.2106(13) 0.2721(9) 0.3637(7) 0.110(6) Uani 1 1 d . . . H25A H 1.2328 0.2845 0.3917 0.132 Uiso 1 1 calc R . . H25B H 1.2287 0.2345 0.3601 0.132 Uiso 1 1 calc R . . C26 C 1.1081(12) 0.2749(8) 0.3639(5) 0.091(5) Uani 1 1 d . . . H26A H 1.0847 0.2487 0.3846 0.110 Uiso 1 1 calc R . . H26B H 1.0893 0.3108 0.3733 0.110 Uiso 1 1 calc R . . N31 N 0.2583(8) 0.6230(5) 0.1622(5) 0.078(3) Uani 1 1 d . . . N32 N 0.2140(7) 0.6361(4) 0.2497(4) 0.069(3) Uani 1 1 d . . . H13N H 0.1732 0.6117 0.2588 0.083 Uiso 1 1 calc R . . H14N H 0.2303 0.6560 0.2729 0.083 Uiso 1 1 calc R . . N33 N 0.4277(7) 0.6490(4) 0.1966(4) 0.064(3) Uani 1 1 d . . . H15N H 0.4257 0.6811 0.2107 0.077 Uiso 1 1 calc R . . H16N H 0.4827 0.6350 0.2002 0.077 Uiso 1 1 calc R . . N34 N 0.2792(9) 0.5138(5) 0.1978(5) 0.090(4) Uani 1 1 d . . . H17N H 0.3257 0.4918 0.1917 0.108 Uiso 1 1 calc R . . H18N H 0.2438 0.4968 0.2172 0.108 Uiso 1 1 calc R . . C31 C 0.1705(11) 0.6426(7) 0.1757(5) 0.090(5) Uani 1 1 d . . . H31A H 0.1300 0.6120 0.1779 0.108 Uiso 1 1 calc R . . H31B H 0.1474 0.6670 0.1535 0.108 Uiso 1 1 calc R . . C32 C 0.1730(11) 0.6714(7) 0.2179(6) 0.090(5) Uani 1 1 d . . . H32A H 0.2072 0.7047 0.2151 0.109 Uiso 1 1 calc R . . H32B H 0.1130 0.6808 0.2270 0.109 Uiso 1 1 calc R . . C33 C 0.3164(11) 0.6632(7) 0.1427(6) 0.090(5) Uani 1 1 d . . . H33A H 0.2971 0.6989 0.1522 0.108 Uiso 1 1 calc R . . H33B H 0.3089 0.6617 0.1113 0.108 Uiso 1 1 calc R . . C34 C 0.4121(10) 0.6575(5) 0.1526(5) 0.075(4) Uani 1 1 d . . . H34A H 0.4361 0.6272 0.1361 0.089 Uiso 1 1 calc R . . H34B H 0.4430 0.6902 0.1434 0.089 Uiso 1 1 calc R . . C35 C 0.2284(14) 0.5261(9) 0.1572(8) 0.130(8) Uani 1 1 d . . . H35A H 0.2333 0.4954 0.1375 0.157 Uiso 1 1 calc R . . H35B H 0.1659 0.5304 0.1645 0.157 Uiso 1 1 calc R . . C36 C 0.2596(15) 0.5755(9) 0.1345(7) 0.119(7) Uani 1 1 d . . . H36A H 0.3199 0.5696 0.1240 0.142 Uiso 1 1 calc R . . H36B H 0.2218 0.5820 0.1093 0.142 Uiso 1 1 calc R . . N41 N 0.5413(10) 0.1936(6) 0.0860(4) 0.090(4) Uani 1 1 d . . . N42 N 0.5128(8) 0.2362(6) 0.1708(5) 0.093(4) Uani 1 1 d . . . H19N H 0.4918 0.2108 0.1893 0.111 Uiso 1 1 calc R . . H20N H 0.5227 0.2666 0.1863 0.111 Uiso 1 1 calc R . . N43 N 0.7082(10) 0.2497(5) 0.0881(4) 0.086(4) Uani 1 1 d . . . H21N H 0.7078 0.2858 0.0930 0.103 Uiso 1 1 calc R . . H22N H 0.7655 0.2389 0.0873 0.103 Uiso 1 1 calc R . . N44 N 0.6483(11) 0.1205(7) 0.1366(5) 0.116(6) Uani 1 1 d . . . H23N H 0.7001 0.1116 0.1236 0.139 Uiso 1 1 calc R . . H24N H 0.6474 0.1049 0.1632 0.139 Uiso 1 1 calc R . . C41 C 0.4513(14) 0.2046(10) 0.1048(7) 0.119(7) Uani 1 1 d . . . H41A H 0.4113 0.2130 0.0808 0.143 Uiso 1 1 calc R . . H41B H 0.4300 0.1713 0.1181 0.143 Uiso 1 1 calc R . . C42 C 0.4430(13) 0.2477(9) 0.1368(6) 0.111(7) Uani 1 1 d . . . H42A H 0.3840 0.2475 0.1498 0.133 Uiso 1 1 calc R . . H42B H 0.4533 0.2829 0.1235 0.133 Uiso 1 1 calc R . . C43 C 0.5686(13) 0.2325(8) 0.0529(5) 0.100(6) Uani 1 1 d . . . H43A H 0.5435 0.2676 0.0604 0.120 Uiso 1 1 calc R . . H43B H 0.5428 0.2216 0.0253 0.120 Uiso 1 1 calc R . . C44 C 0.6682(12) 0.2393(8) 0.0467(5) 0.094(5) Uani 1 1 d . . . H44A H 0.6933 0.2066 0.0341 0.113 Uiso 1 1 calc R . . H44B H 0.6799 0.2694 0.0270 0.113 Uiso 1 1 calc R . . C45 C 0.5480(15) 0.1356(9) 0.0722(6) 0.111(6) Uani 1 1 d . . . H45A H 0.5932 0.1321 0.0498 0.133 Uiso 1 1 calc R . . H45B H 0.4914 0.1240 0.0600 0.133 Uiso 1 1 calc R . . C46 C 0.5713(14) 0.0999(9) 0.1099(7) 0.115(7) Uani 1 1 d . . . H46A H 0.5860 0.0640 0.0989 0.139 Uiso 1 1 calc R . . H46B H 0.5195 0.0963 0.1286 0.139 Uiso 1 1 calc R . . N51 N 0.5954(10) 0.4423(6) 0.0135(4) 0.098(5) Uani 1 1 d D . . N52 N 0.6201(11) 0.5225(6) -0.0528(4) 0.109(5) Uani 1 1 d D . . H25N H 0.6100 0.5575 -0.0595 0.130 Uiso 1 1 calc R . . H26N H 0.6553 0.5082 -0.0736 0.130 Uiso 1 1 calc R . . N53 N 0.5741(12) 0.5442(7) 0.0541(5) 0.121(6) Uani 1 1 d D . . H27N H 0.5949 0.5516 0.0810 0.145 Uiso 1 1 calc R . . H28N H 0.5511 0.5750 0.0431 0.145 Uiso 1 1 calc R . . N54 N 0.7803(12) 0.4495(8) -0.0097(5) 0.122(6) Uani 1 1 d D . . H29N H 0.8066 0.4587 -0.0350 0.146 Uiso 1 1 calc R . . H30N H 0.8233 0.4448 0.0104 0.146 Uiso 1 1 calc R . . C51 C 0.5438(14) 0.4402(7) -0.0271(5) 0.109(7) Uani 1 1 d D . . H51A H 0.4845 0.4268 -0.0204 0.131 Uiso 1 1 calc R . . H51B H 0.5717 0.4140 -0.0464 0.131 Uiso 1 1 calc R . . C52 C 0.5344(12) 0.4927(8) -0.0513(6) 0.120(8) Uani 1 1 d D . . H52A H 0.5144 0.4854 -0.0808 0.143 Uiso 1 1 calc R . . H52B H 0.4897 0.5150 -0.0372 0.143 Uiso 1 1 calc R . . C53 C 0.5420(16) 0.4491(9) 0.0517(6) 0.128(8) Uani 1 1 d D . . H53A H 0.5779 0.4403 0.0771 0.154 Uiso 1 1 calc R . . H53B H 0.4930 0.4235 0.0507 0.154 Uiso 1 1 calc R . . C54 C 0.5052(13) 0.5045(9) 0.0573(6) 0.133(10) Uani 1 1 d D . . H54A H 0.4606 0.5113 0.0351 0.160 Uiso 1 1 calc R . . H54B H 0.4765 0.5073 0.0856 0.160 Uiso 1 1 calc R . . C55 C 0.6567(16) 0.3955(7) 0.0189(8) 0.131(9) Uani 1 1 d D . . H55A H 0.6240 0.3618 0.0153 0.158 Uiso 1 1 calc R . . H55B H 0.6823 0.3958 0.0480 0.158 Uiso 1 1 calc R . . C56 C 0.7316(19) 0.3989(9) -0.0154(9) 0.177(13) Uani 1 1 d D . . H56A H 0.7719 0.3684 -0.0120 0.212 Uiso 1 1 calc R . . H56B H 0.7062 0.3975 -0.0444 0.212 Uiso 1 1 calc R . . N61 N 0.7912(18) 0.7121(10) -0.0089(8) 0.164(8) Uiso 1 1 d . . . N62 N 0.7761(13) 0.5888(7) 0.0049(6) 0.128(6) Uiso 1 1 d . . . H31N H 0.8333 0.5777 0.0054 0.154 Uiso 1 1 calc R . . H32N H 0.7660 0.6044 -0.0212 0.154 Uiso 1 1 calc R . . N63 N 0.9054(12) 0.6967(7) -0.0928(5) 0.115(5) Uiso 1 1 d . . . H33N H 0.9503 0.6801 -0.1063 0.172 Uiso 1 1 calc R . . H34N H 0.8870 0.7247 -0.1088 0.172 Uiso 1 1 calc R . . H35N H 0.8606 0.6734 -0.0892 0.172 Uiso 1 1 calc R . . N64 N 0.617(2) 0.6890(12) -0.0625(9) 0.212(12) Uiso 1 1 d . . . H36N H 0.6567 0.6623 -0.0644 0.318 Uiso 1 1 calc R . . H37N H 0.5897 0.6931 -0.0881 0.318 Uiso 1 1 calc R . . H38N H 0.5768 0.6810 -0.0422 0.318 Uiso 1 1 calc R . . C61 C 0.8136(19) 0.6808(11) 0.0309(9) 0.152(9) Uiso 1 1 d . . . H61A H 0.8764 0.6715 0.0295 0.182 Uiso 1 1 calc R . . H61B H 0.8058 0.7047 0.0558 0.182 Uiso 1 1 calc R . . C62 C 0.7630(16) 0.6303(9) 0.0396(7) 0.125(7) Uiso 1 1 d . . . H62A H 0.7000 0.6388 0.0418 0.150 Uiso 1 1 calc R . . H62B H 0.7819 0.6153 0.0674 0.150 Uiso 1 1 calc R . . C63 C 0.874(3) 0.7507(16) -0.0250(13) 0.224(16) Uiso 1 1 d . . . H63A H 0.8519 0.7792 -0.0440 0.269 Uiso 1 1 calc R . . H63B H 0.9025 0.7674 0.0000 0.269 Uiso 1 1 calc R . . C64 C 0.937(2) 0.7172(14) -0.0481(11) 0.191(13) Uiso 1 1 d . . . H64A H 0.9512 0.6860 -0.0301 0.229 Uiso 1 1 calc R . . H64B H 0.9914 0.7378 -0.0522 0.229 Uiso 1 1 calc R . . C65 C 0.704(3) 0.7457(16) -0.0081(13) 0.208(14) Uiso 1 1 d . . . H65A H 0.6656 0.7336 0.0154 0.249 Uiso 1 1 calc R . . H65B H 0.7172 0.7839 -0.0039 0.249 Uiso 1 1 calc R . . C66 C 0.660(2) 0.7366(15) -0.0516(11) 0.194(13) Uiso 1 1 d . . . H66A H 0.6164 0.7655 -0.0551 0.233 Uiso 1 1 calc R . . H66B H 0.7052 0.7425 -0.0736 0.233 Uiso 1 1 calc R . . O49 O 0.7427(15) 0.4607(9) 0.2436(7) 0.087(6) Uiso 0.50 1 d P . . O50 O 0.3752(18) 0.3993(10) 0.1266(8) 0.104(7) Uiso 0.50 1 d P . . O51 O 0.506(2) 0.6510(12) -0.0020(9) 0.097(9) Uiso 0.40 1 d P . . O52 O 0.999(3) 0.5022(16) 0.0634(12) 0.135(13) Uiso 0.40 1 d P . . O53 O 0.551(3) 0.4698(16) 0.4560(12) 0.131(12) Uiso 0.40 1 d P . . O54 O 1.136(4) 0.525(2) 0.3640(17) 0.137(17) Uiso 0.30 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.0470(7) 0.0465(6) 0.0508(7) -0.0004(5) 0.0035(6) -0.0058(5) Ge2 0.0463(7) 0.0332(5) 0.0551(7) 0.0007(5) -0.0027(6) -0.0031(5) Ge3 0.0495(7) 0.0350(6) 0.0510(7) -0.0005(5) -0.0014(6) 0.0003(5) Ge4 0.0465(6) 0.0368(6) 0.0525(7) -0.0001(5) -0.0004(5) 0.0030(5) Ge5 0.0455(6) 0.0398(6) 0.0527(7) 0.0011(5) 0.0030(5) -0.0018(5) Ge6 0.0433(6) 0.0435(6) 0.0508(7) -0.0036(5) 0.0014(5) 0.0026(5) V1 0.0446(10) 0.0401(9) 0.0575(12) -0.0001(9) -0.0029(9) 0.0012(8) V2 0.0475(11) 0.0386(9) 0.0510(11) -0.0033(8) -0.0007(9) 0.0013(8) V3 0.0493(11) 0.0400(9) 0.0438(10) 0.0009(8) -0.0003(8) -0.0023(8) V4 0.0467(11) 0.0399(9) 0.0520(11) -0.0005(8) 0.0001(9) -0.0037(8) V5 0.0464(10) 0.0360(9) 0.0461(10) 0.0002(8) -0.0012(8) 0.0010(8) V6 0.0500(11) 0.0358(9) 0.0521(11) 0.0009(8) -0.0001(9) -0.0060(8) V7 0.0501(11) 0.0395(9) 0.0510(11) -0.0007(8) -0.0043(9) -0.0019(8) V8 0.0491(11) 0.0372(9) 0.0501(11) 0.0015(8) 0.0001(9) -0.0004(8) V9 0.0424(10) 0.0392(9) 0.0612(12) 0.0001(9) -0.0027(9) -0.0038(8) V10 0.0420(10) 0.0392(9) 0.0584(12) 0.0019(8) 0.0023(9) 0.0036(8) V11 0.0507(11) 0.0419(10) 0.0482(11) -0.0039(8) 0.0012(9) -0.0002(9) V12 0.0490(11) 0.0379(9) 0.0473(11) -0.0022(8) -0.0027(9) 0.0022(8) V13 0.0484(11) 0.0401(9) 0.0464(10) -0.0007(8) 0.0017(9) 0.0015(8) V14 0.0443(10) 0.0368(9) 0.0492(11) 0.0003(8) -0.0021(8) 0.0011(8) V15 0.0455(10) 0.0374(9) 0.0495(11) -0.0001(8) -0.0022(8) 0.0003(8) O1 0.051(4) 0.047(4) 0.054(5) -0.001(4) 0.000(4) 0.000(4) O2 0.047(5) 0.064(5) 0.089(7) 0.001(5) -0.004(5) -0.005(4) O3 0.060(5) 0.072(6) 0.077(6) 0.010(5) 0.008(5) 0.000(5) O4 0.055(5) 0.053(5) 0.092(7) -0.004(5) 0.018(5) 0.002(4) O5 0.050(4) 0.047(4) 0.050(4) -0.007(4) 0.002(4) -0.009(4) O6 0.049(5) 0.058(5) 0.049(4) -0.006(4) 0.001(4) -0.012(4) O7 0.052(5) 0.052(4) 0.053(5) -0.002(4) -0.006(4) -0.007(4) O8 0.046(4) 0.066(5) 0.076(6) 0.011(4) -0.019(4) -0.001(4) O9 0.054(5) 0.056(5) 0.055(5) -0.001(4) -0.001(4) -0.009(4) O10 0.074(6) 0.072(6) 0.056(5) 0.007(4) 0.007(5) -0.023(5) O11 0.061(5) 0.066(5) 0.070(6) 0.000(5) -0.002(5) 0.006(4) O12 0.041(4) 0.030(3) 0.084(6) 0.004(4) 0.012(4) -0.003(3) O13 0.057(5) 0.033(4) 0.064(5) 0.006(3) -0.001(4) -0.003(3) O14 0.056(5) 0.068(5) 0.055(5) -0.012(4) -0.001(4) 0.001(4) O15 0.059(5) 0.031(4) 0.070(5) 0.001(4) -0.004(4) 0.004(3) O16 0.088(6) 0.044(4) 0.058(5) 0.013(4) -0.005(5) -0.008(4) O17 0.044(4) 0.054(4) 0.067(5) 0.008(4) -0.006(4) 0.015(4) O18 0.044(4) 0.047(4) 0.054(5) -0.003(3) -0.002(4) -0.010(3) O19 0.056(5) 0.027(3) 0.083(6) -0.005(4) -0.007(4) 0.003(3) O20 0.054(5) 0.039(4) 0.052(5) 0.004(3) -0.012(4) 0.002(3) O21 0.060(5) 0.053(5) 0.067(5) -0.009(4) 0.001(4) 0.018(4) O22 0.051(5) 0.046(4) 0.057(5) -0.004(4) -0.006(4) 0.003(4) O23 0.067(5) 0.040(4) 0.078(6) 0.013(4) -0.003(5) -0.016(4) O24 0.063(5) 0.047(4) 0.060(5) -0.009(4) -0.004(4) -0.001(4) O25 0.069(6) 0.065(5) 0.052(5) -0.004(4) 0.002(4) -0.006(5) O26 0.042(4) 0.059(5) 0.052(5) -0.004(4) 0.004(4) -0.010(4) O27 0.051(5) 0.045(4) 0.053(5) 0.000(4) -0.008(4) -0.009(3) O28 0.038(4) 0.045(4) 0.059(5) 0.002(4) 0.000(3) 0.005(3) O29 0.049(4) 0.041(4) 0.050(4) 0.007(3) 0.005(4) -0.004(3) O30 0.047(4) 0.039(4) 0.049(4) -0.003(3) -0.002(3) 0.001(3) O31 0.045(4) 0.031(3) 0.062(5) 0.006(3) -0.007(4) -0.006(3) O32 0.054(5) 0.045(4) 0.046(4) 0.000(3) 0.003(4) 0.004(4) O33 0.058(5) 0.053(5) 0.064(5) 0.005(4) -0.012(4) -0.009(4) O34 0.048(4) 0.052(4) 0.051(4) -0.005(4) 0.002(4) -0.004(4) O35 0.051(4) 0.043(4) 0.053(4) 0.001(3) -0.003(4) -0.001(3) O36 0.053(5) 0.057(5) 0.047(4) 0.000(4) 0.002(4) -0.013(4) O37 0.051(5) 0.042(4) 0.058(5) -0.003(3) 0.000(4) 0.004(3) O38 0.057(5) 0.039(4) 0.054(4) 0.002(3) 0.001(4) -0.003(3) O39 0.056(5) 0.036(4) 0.054(4) 0.001(3) 0.007(4) -0.004(3) O40 0.049(4) 0.045(4) 0.057(5) 0.007(4) -0.003(4) 0.002(3) O41 0.041(4) 0.053(4) 0.048(4) -0.001(4) 0.001(3) -0.001(3) O42 0.046(4) 0.041(4) 0.058(5) 0.001(3) -0.005(4) 0.006(3) O43 0.072(6) 0.034(4) 0.069(5) 0.009(4) -0.015(5) 0.005(4) O44 0.054(5) 0.049(4) 0.047(4) -0.005(3) -0.002(4) 0.000(4) O45 0.056(5) 0.040(4) 0.048(4) -0.002(3) -0.003(4) 0.001(3) O46 0.044(4) 0.031(3) 0.061(5) -0.005(3) -0.005(4) 0.010(3) O47 0.038(4) 0.045(4) 0.059(5) -0.006(4) 0.002(4) -0.002(3) O48 0.046(4) 0.055(4) 0.048(4) -0.001(4) -0.005(4) -0.004(4) Mn1 0.0670(12) 0.0466(9) 0.0553(11) 0.0003(8) 0.0015(9) 0.0088(9) Mn2 0.0486(10) 0.0448(9) 0.0608(11) -0.0015(8) -0.0060(9) 0.0020(8) Mn3 0.0613(12) 0.0492(10) 0.0901(15) 0.0099(10) -0.0178(11) -0.0064(9) Mn4 0.0848(17) 0.0974(17) 0.0722(15) -0.0034(13) -0.0037(13) -0.0268(14) Mn5 0.0889(17) 0.0761(14) 0.0691(14) -0.0003(11) -0.0045(12) -0.0059(13) N11 0.079(9) 0.078(8) 0.073(8) 0.005(6) 0.008(7) 0.014(7) N13 0.117(11) 0.068(8) 0.096(10) 0.002(7) 0.032(9) 0.006(8) N14 0.065(7) 0.059(6) 0.079(8) 0.000(6) 0.006(6) 0.022(5) C11 0.133(19) 0.24(3) 0.080(13) 0.014(16) 0.004(13) 0.10(2) C12 0.082(11) 0.062(8) 0.096(11) -0.004(8) 0.027(9) 0.012(8) C13 0.115(16) 0.097(13) 0.122(16) 0.048(12) 0.051(13) 0.018(12) C14 0.124(16) 0.092(12) 0.092(13) 0.005(10) 0.049(12) 0.005(12) C15 0.107(14) 0.125(15) 0.069(10) 0.004(10) -0.020(10) 0.053(12) C16 0.079(11) 0.083(11) 0.110(13) -0.031(10) -0.052(10) 0.022(9) N21 0.060(7) 0.086(8) 0.070(8) -0.004(7) -0.002(6) 0.003(6) N22 0.056(6) 0.032(5) 0.091(8) -0.010(5) -0.011(6) 0.004(4) N23 0.071(7) 0.056(6) 0.085(8) 0.002(6) 0.000(6) -0.011(6) N24 0.061(7) 0.065(6) 0.061(7) 0.001(5) 0.003(5) 0.013(5) C21 0.072(10) 0.113(13) 0.081(11) -0.025(10) -0.027(8) 0.027(9) C22 0.054(8) 0.053(7) 0.142(15) -0.009(9) -0.024(9) 0.010(6) C23 0.051(8) 0.088(10) 0.093(11) -0.031(9) -0.013(8) 0.003(7) C24 0.060(8) 0.041(6) 0.114(12) -0.016(7) -0.016(8) -0.010(6) C25 0.094(14) 0.131(17) 0.104(14) 0.008(13) -0.027(12) 0.006(12) C26 0.104(13) 0.110(13) 0.060(9) -0.013(9) 0.018(9) -0.027(11) N31 0.055(7) 0.080(8) 0.100(9) -0.003(7) -0.022(7) -0.003(6) N32 0.058(7) 0.056(6) 0.094(9) 0.015(6) -0.004(6) -0.005(5) N33 0.048(6) 0.041(5) 0.104(10) -0.002(6) 0.001(6) -0.008(4) N34 0.082(9) 0.050(6) 0.138(13) 0.003(7) 0.012(9) -0.004(6) C31 0.090(12) 0.086(10) 0.093(12) 0.007(9) -0.044(10) -0.004(9) C32 0.066(10) 0.105(12) 0.101(12) -0.012(10) -0.005(9) 0.024(9) C33 0.082(11) 0.082(10) 0.104(12) 0.029(9) -0.021(10) -0.014(9) C34 0.081(10) 0.049(7) 0.094(12) 0.005(7) 0.020(9) -0.015(7) C35 0.105(16) 0.122(17) 0.16(2) -0.025(16) 0.004(15) -0.075(14) C36 0.107(15) 0.130(17) 0.119(16) -0.032(14) -0.018(13) 0.020(14) N41 0.088(10) 0.101(10) 0.079(9) -0.003(8) -0.009(8) -0.022(8) N42 0.070(8) 0.102(10) 0.106(11) 0.004(8) 0.017(8) -0.036(7) N43 0.110(11) 0.085(9) 0.063(7) 0.005(6) 0.009(7) -0.031(8) N44 0.108(12) 0.128(13) 0.112(12) -0.022(10) 0.011(10) -0.054(11) C41 0.102(15) 0.16(2) 0.098(14) 0.000(14) 0.005(12) -0.033(14) C42 0.093(14) 0.146(18) 0.094(13) -0.022(13) -0.011(11) -0.025(13) C43 0.109(14) 0.123(15) 0.067(10) 0.009(10) -0.021(10) -0.030(12) C44 0.102(13) 0.110(13) 0.069(10) 0.001(9) 0.001(10) -0.027(11) C45 0.117(16) 0.128(16) 0.088(12) -0.016(12) 0.018(12) -0.032(14) C46 0.119(16) 0.126(16) 0.101(14) 0.005(12) -0.007(12) -0.065(13) N51 0.113(12) 0.105(11) 0.076(9) -0.009(8) 0.002(8) -0.039(9) N52 0.140(14) 0.108(11) 0.077(9) 0.001(8) 0.008(9) -0.037(11) N53 0.129(14) 0.132(14) 0.101(12) -0.018(10) -0.037(11) 0.032(12) N54 0.112(13) 0.164(16) 0.089(11) -0.041(11) 0.011(9) -0.030(12) C51 0.129(16) 0.124(16) 0.074(11) 0.014(10) -0.004(11) -0.068(13) C52 0.097(14) 0.20(2) 0.066(10) -0.013(13) 0.014(10) -0.030(15) C53 0.17(2) 0.123(17) 0.096(14) -0.033(13) 0.031(15) -0.023(17) C54 0.105(15) 0.23(3) 0.066(11) -0.055(15) 0.022(10) -0.046(18) C55 0.19(3) 0.051(9) 0.148(19) 0.003(11) 0.038(19) 0.024(13) C56 0.27(4) 0.111(19) 0.15(2) -0.057(17) -0.03(3) 0.02(2) _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 O10 1.721(8) . ? Ge1 O29 1.734(7) . ? Ge1 O48 1.744(7) . ? Ge1 O22 1.752(8) . ? Ge2 O37 1.708(7) . ? Ge2 O47 1.748(7) . ? Ge2 O15 1.753(7) . ? Ge2 O31 1.759(8) . ? Ge3 O19 1.699(7) . ? Ge3 O27 1.748(8) . ? Ge3 O41 1.760(7) . ? Ge3 O20 1.768(8) . ? Ge4 O42 1.707(7) . ? Ge4 O45 1.742(7) . ? Ge4 O7 1.747(8) . ? Ge4 O20 1.763(7) . ? Ge5 O3 1.722(9) . ? Ge5 O18 1.745(7) . ? Ge5 O31 1.751(7) . ? Ge5 O13 1.765(7) . ? Ge6 O11 1.685(8) . ? Ge6 O38 1.749(8) . ? Ge6 O5 1.750(8) . ? Ge6 O29 1.784(7) . ? V1 O8 1.607(8) . ? V1 O35 1.908(8) . ? V1 O40 1.936(8) . ? V1 O12 1.963(8) . ? V1 O7 2.042(8) . ? V1 V9 2.904(3) . ? V1 V8 3.060(3) . ? V2 O21 1.606(7) . ? V2 O1 1.916(8) . ? V2 O28 1.943(8) . ? V2 O5 1.999(8) . ? V2 O47 2.004(8) . ? V2 V11 3.018(3) . ? V2 V15 3.037(3) . ? V3 O6 1.567(8) . ? V3 O35 1.924(8) . ? V3 O34 1.942(8) . ? V3 O26 1.944(8) . ? V3 O22 2.015(8) . ? V3 V8 2.869(3) . ? V3 V11 3.056(3) . ? V4 O33 1.616(8) . ? V4 O39 1.909(7) . ? V4 O36 1.939(8) . ? V4 O38 2.007(7) . ? V4 O48 2.014(8) . ? V4 V12 2.876(3) . ? V4 V6 3.037(3) . ? V4 V14 3.053(3) . ? V5 O32 1.603(8) . ? V5 O46 1.888(7) . ? V5 O44 1.910(8) . ? V5 O30 1.942(8) . ? V5 O18 2.004(7) . ? V5 V13 2.846(3) . ? V5 V15 3.057(3) . ? V6 O23 1.600(7) . ? V6 O26 1.930(8) . ? V6 O36 1.954(8) . ? V6 O27 1.991(8) . ? V6 O48 2.005(8) . ? V6 V8 3.035(3) . ? V7 O9 1.592(8) . ? V7 O40 1.914(8) . ? V7 O34 1.943(8) . ? V7 O1 1.944(8) . ? V7 O15 2.065(8) . ? V7 V11 2.869(3) . ? V7 V9 3.066(3) . ? V8 O16 1.619(8) . ? V8 O35 1.915(7) . ? V8 O26 1.937(8) . ? V8 O27 1.994(8) . ? V8 O7 2.029(8) . ? V9 O2 1.626(8) . ? V9 O40 1.884(8) . ? V9 O12 1.939(7) . ? V9 O13 1.983(8) . ? V9 O15 2.051(7) . ? V9 V10 3.036(3) . ? V10 O4 1.588(9) . ? V10 O12 1.920(9) . ? V10 O30 1.955(8) . ? V10 O45 1.989(7) . ? V10 O13 2.005(7) . ? V10 V13 3.028(3) . ? V11 O14 1.583(8) . ? V11 O34 1.900(8) . ? V11 O1 1.938(8) . ? V11 O22 1.987(8) . ? V11 O5 1.996(8) . ? V12 O24 1.588(8) . ? V12 O39 1.902(7) . ? V12 O46 1.947(8) . ? V12 O36 1.950(8) . ? V12 O41 2.027(8) . ? V12 V13 3.065(3) . ? V13 O25 1.587(8) . ? V13 O30 1.921(7) . ? V13 O46 1.922(7) . ? V13 O41 1.984(8) . ? V13 O45 2.033(8) . ? V14 O17 1.589(8) . ? V14 O39 1.942(7) . ? V14 O44 1.947(8) . ? V14 O28 1.949(8) . ? V14 O38 2.014(8) . ? V14 V15 2.873(3) . ? V15 O43 1.591(7) . ? V15 O44 1.929(7) . ? V15 O28 1.940(8) . ? V15 O47 2.001(8) . ? V15 O18 2.018(8) . ? O11 Mn3 2.026(9) . ? O19 Mn4 1.992(9) . ? O32 Mn5 2.258(8) . ? O37 Mn1 2.109(8) 3_755 ? O37 Mn2 2.297(7) 3_755 ? O42 Mn2 2.141(8) . ? O42 Mn1 2.196(8) . ? Mn1 O37 2.109(8) 3_745 ? Mn1 N12 2.246(12) . ? Mn1 N14 2.251(12) . ? Mn1 N11 2.316(13) . ? Mn1 N13 2.518(13) . ? Mn1 Mn2 3.145(3) . ? Mn2 N24 2.236(11) . ? Mn2 N22 2.281(10) . ? Mn2 O37 2.297(7) 3_745 ? Mn2 N23 2.330(10) . ? Mn2 N21 2.368(12) . ? Mn3 N32 2.146(11) . ? Mn3 N33 2.214(10) . ? Mn3 N34 2.257(13) . ? Mn3 N31 2.335(13) . ? Mn4 N44 2.164(17) . ? Mn4 N42 2.190(14) . ? Mn4 N43 2.237(12) . ? Mn4 N41 2.321(14) . ? Mn5 N62 2.213(18) . ? Mn5 N52 2.229(15) . ? Mn5 N53 2.250(18) . ? Mn5 N54 2.258(19) . ? Mn5 N51 2.308(14) . ? N11 C11 1.50(2) . ? N11 C13 1.52(2) . ? N11 C15 1.55(2) . ? N12 C12 1.545(19) . ? N13 C14 1.50(2) . ? N14 C16 1.520(18) . ? C11 C12 1.50(3) . ? C13 C14 1.42(3) . ? C15 C16 1.45(2) . ? N21 C25 1.40(2) . ? N21 C23 1.494(19) . ? N21 C21 1.497(18) . ? N22 C22 1.513(18) . ? N23 C24 1.440(17) . ? N24 C26 1.484(18) . ? C21 C22 1.51(2) . ? C23 C24 1.43(2) . ? C25 C26 1.54(2) . ? N31 C33 1.446(19) . ? N31 C36 1.45(2) . ? N31 C31 1.46(2) . ? N32 C32 1.444(19) . ? N33 C34 1.387(18) . ? N34 C35 1.49(3) . ? C31 C32 1.48(2) . ? C33 C34 1.47(2) . ? C35 C36 1.48(3) . ? N41 C43 1.46(2) . ? N41 C45 1.49(2) . ? N41 C41 1.49(2) . ? N42 C42 1.50(2) . ? N43 C44 1.427(19) . ? N44 C46 1.50(2) . ? C41 C42 1.45(3) . ? C43 C44 1.51(2) . ? C45 C46 1.49(3) . ? N51 C53 1.428(16) . ? N51 C51 1.469(15) . ? N51 C55 1.485(16) . ? N52 C52 1.480(15) . ? N53 C54 1.425(16) . ? N54 C56 1.454(16) . ? C51 C52 1.496(16) . ? C53 C54 1.481(17) . ? C55 C56 1.539(18) . ? N61 C61 1.48(3) . ? N61 C65 1.55(4) . ? N61 C63 1.64(4) . ? N62 C62 1.49(2) . ? N63 C64 1.53(3) . ? N64 C66 1.38(4) . ? C61 C62 1.48(3) . ? C63 C64 1.44(4) . ? C65 C66 1.51(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 Ge1 O29 107.6(4) . . ? O10 Ge1 O48 112.1(4) . . ? O29 Ge1 O48 107.7(4) . . ? O10 Ge1 O22 113.3(4) . . ? O29 Ge1 O22 106.6(3) . . ? O48 Ge1 O22 109.2(4) . . ? O37 Ge2 O47 112.2(4) . . ? O37 Ge2 O15 118.8(4) . . ? O47 Ge2 O15 106.0(4) . . ? O37 Ge2 O31 108.7(3) . . ? O47 Ge2 O31 104.3(3) . . ? O15 Ge2 O31 105.7(4) . . ? O19 Ge3 O27 114.9(4) . . ? O19 Ge3 O41 115.0(4) . . ? O27 Ge3 O41 106.4(3) . . ? O19 Ge3 O20 109.6(4) . . ? O27 Ge3 O20 104.0(4) . . ? O41 Ge3 O20 106.1(3) . . ? O42 Ge4 O45 113.7(4) . . ? O42 Ge4 O7 115.0(4) . . ? O45 Ge4 O7 107.6(4) . . ? O42 Ge4 O20 108.1(3) . . ? O45 Ge4 O20 105.1(3) . . ? O7 Ge4 O20 106.7(4) . . ? O3 Ge5 O18 113.6(4) . . ? O3 Ge5 O31 109.0(4) . . ? O18 Ge5 O31 106.7(3) . . ? O3 Ge5 O13 112.1(4) . . ? O18 Ge5 O13 108.7(4) . . ? O31 Ge5 O13 106.5(3) . . ? O11 Ge6 O38 114.5(4) . . ? O11 Ge6 O5 114.5(4) . . ? O38 Ge6 O5 106.5(4) . . ? O11 Ge6 O29 111.0(4) . . ? O38 Ge6 O29 105.2(3) . . ? O5 Ge6 O29 104.3(4) . . ? O8 V1 O35 108.3(4) . . ? O8 V1 O40 106.4(4) . . ? O35 V1 O40 91.1(3) . . ? O8 V1 O12 110.9(4) . . ? O35 V1 O12 140.7(3) . . ? O40 V1 O12 80.1(3) . . ? O8 V1 O7 106.0(4) . . ? O35 V1 O7 78.0(3) . . ? O40 V1 O7 147.6(3) . . ? O12 V1 O7 89.3(3) . . ? O8 V1 V9 106.5(3) . . ? O35 V1 V9 126.3(2) . . ? O40 V1 V9 39.9(2) . . ? O12 V1 V9 41.6(2) . . ? O7 V1 V9 128.4(2) . . ? O8 V1 V8 111.5(3) . . ? O35 V1 V8 36.9(2) . . ? O40 V1 V8 122.5(2) . . ? O12 V1 V8 121.4(2) . . ? O7 V1 V8 41.1(2) . . ? V9 V1 V8 141.92(9) . . ? O21 V2 O1 110.7(4) . . ? O21 V2 O28 113.0(4) . . ? O1 V2 O28 136.3(3) . . ? O21 V2 O5 105.5(4) . . ? O1 V2 O5 79.5(3) . . ? O28 V2 O5 89.3(3) . . ? O21 V2 O47 105.3(4) . . ? O1 V2 O47 89.4(3) . . ? O28 V2 O47 79.0(3) . . ? O5 V2 O47 149.2(3) . . ? O21 V2 V11 111.8(3) . . ? O1 V2 V11 38.7(2) . . ? O28 V2 V11 119.8(2) . . ? O5 V2 V11 40.9(2) . . ? O47 V2 V11 123.8(2) . . ? O21 V2 V15 112.5(3) . . ? O1 V2 V15 120.2(2) . . ? O28 V2 V15 38.5(2) . . ? O5 V2 V15 123.9(2) . . ? O47 V2 V15 40.6(2) . . ? V11 V2 V15 135.61(8) . . ? O6 V3 O35 108.2(4) . . ? O6 V3 O34 108.2(4) . . ? O35 V3 O34 89.2(3) . . ? O6 V3 O26 109.8(4) . . ? O35 V3 O26 82.4(3) . . ? O34 V3 O26 141.9(3) . . ? O6 V3 O22 106.8(4) . . ? O35 V3 O22 144.8(3) . . ? O34 V3 O22 76.6(3) . . ? O26 V3 O22 89.2(3) . . ? O6 V3 V8 107.3(3) . . ? O35 V3 V8 41.5(2) . . ? O34 V3 V8 126.3(2) . . ? O26 V3 V8 42.3(2) . . ? O22 V3 V8 127.9(2) . . ? O6 V3 V11 110.4(3) . . ? O35 V3 V11 120.9(2) . . ? O34 V3 V11 36.8(2) . . ? O26 V3 V11 122.1(3) . . ? O22 V3 V11 39.9(2) . . ? V8 V3 V11 142.30(8) . . ? O33 V4 O39 110.2(4) . . ? O33 V4 O36 110.5(4) . . ? O39 V4 O36 82.5(3) . . ? O33 V4 O38 110.2(4) . . ? O39 V4 O38 78.5(3) . . ? O36 V4 O38 138.9(3) . . ? O33 V4 O48 110.0(4) . . ? O39 V4 O48 139.5(3) . . ? O36 V4 O48 79.7(3) . . ? O38 V4 O48 91.7(3) . . ? O33 V4 V12 111.0(3) . . ? O39 V4 V12 40.9(2) . . ? O36 V4 V12 42.4(2) . . ? O38 V4 V12 115.0(2) . . ? O48 V4 V12 117.4(2) . . ? O33 V4 V6 116.1(3) . . ? O39 V4 V6 113.9(2) . . ? O36 V4 V6 38.9(2) . . ? O38 V4 V6 121.8(2) . . ? O48 V4 V6 40.8(2) . . ? V12 V4 V6 78.89(7) . . ? O33 V4 V14 114.2(3) . . ? O39 V4 V14 37.9(2) . . ? O36 V4 V14 114.1(2) . . ? O38 V4 V14 40.7(2) . . ? O48 V4 V14 123.3(2) . . ? V12 V4 V14 76.99(7) . . ? V6 V4 V14 129.14(8) . . ? O32 V5 O46 104.9(4) . . ? O32 V5 O44 109.2(4) . . ? O46 V5 O44 89.1(3) . . ? O32 V5 O30 108.8(4) . . ? O46 V5 O30 83.2(3) . . ? O44 V5 O30 141.9(3) . . ? O32 V5 O18 107.7(4) . . ? O46 V5 O18 147.3(3) . . ? O44 V5 O18 78.1(3) . . ? O30 V5 O18 88.6(3) . . ? O32 V5 V13 105.0(3) . . ? O46 V5 V13 42.1(2) . . ? O44 V5 V13 126.4(2) . . ? O30 V5 V13 42.3(2) . . ? O18 V5 V13 127.9(2) . . ? O32 V5 V15 112.6(3) . . ? O46 V5 V15 121.7(2) . . ? O44 V5 V15 37.4(2) . . ? O30 V5 V15 121.6(2) . . ? O18 V5 V15 40.7(2) . . ? V13 V5 V15 142.43(8) . . ? O23 V6 O26 112.1(4) . . ? O23 V6 O36 113.0(4) . . ? O26 V6 O36 135.0(3) . . ? O23 V6 O27 104.9(4) . . ? O26 V6 O27 78.6(3) . . ? O36 V6 O27 89.6(3) . . ? O23 V6 O48 104.8(4) . . ? O26 V6 O48 89.7(3) . . ? O36 V6 O48 79.5(3) . . ? O27 V6 O48 150.3(3) . . ? O23 V6 V8 111.1(3) . . ? O26 V6 V8 38.4(2) . . ? O36 V6 V8 119.9(2) . . ? O27 V6 V8 40.4(2) . . ? O48 V6 V8 124.7(2) . . ? O23 V6 V4 114.3(3) . . ? O26 V6 V4 118.4(3) . . ? O36 V6 V4 38.5(2) . . ? O27 V6 V4 123.4(2) . . ? O48 V6 V4 41.0(2) . . ? V8 V6 V4 134.57(8) . . ? O9 V7 O40 110.8(4) . . ? O9 V7 O34 106.8(4) . . ? O40 V7 O34 90.4(3) . . ? O9 V7 O1 110.1(4) . . ? O40 V7 O1 138.9(3) . . ? O34 V7 O1 82.2(3) . . ? O9 V7 O15 103.8(4) . . ? O40 V7 O15 77.4(3) . . ? O34 V7 O15 149.4(3) . . ? O1 V7 O15 88.7(3) . . ? O9 V7 V11 107.0(3) . . ? O40 V7 V11 125.6(2) . . ? O34 V7 V11 41.1(2) . . ? O1 V7 V11 42.3(2) . . ? O15 V7 V11 128.6(2) . . ? O9 V7 V9 111.1(3) . . ? O40 V7 V9 35.8(2) . . ? O34 V7 V9 122.2(2) . . ? O1 V7 V9 121.1(2) . . ? O15 V7 V9 41.7(2) . . ? V11 V7 V9 141.88(9) . . ? O16 V8 O35 111.6(4) . . ? O16 V8 O26 111.8(4) . . ? O35 V8 O26 82.8(3) . . ? O16 V8 O27 110.8(4) . . ? O35 V8 O27 137.4(3) . . ? O26 V8 O27 78.4(3) . . ? O16 V8 O7 106.0(4) . . ? O35 V8 O7 78.2(3) . . ? O26 V8 O7 141.8(3) . . ? O27 V8 O7 93.8(3) . . ? O16 V8 V3 111.2(3) . . ? O35 V8 V3 41.8(2) . . ? O26 V8 V3 42.4(2) . . ? O27 V8 V3 116.4(2) . . ? O7 V8 V3 117.2(2) . . ? O16 V8 V6 114.9(3) . . ? O35 V8 V6 114.4(2) . . ? O26 V8 V6 38.2(2) . . ? O27 V8 V6 40.4(2) . . ? O7 V8 V6 126.3(2) . . ? V3 V8 V6 79.03(7) . . ? O16 V8 V1 113.9(3) . . ? O35 V8 V1 36.8(2) . . ? O26 V8 V1 113.8(2) . . ? O27 V8 V1 123.1(2) . . ? O7 V8 V1 41.4(2) . . ? V3 V8 V1 77.18(7) . . ? V6 V8 V1 130.64(8) . . ? O2 V9 O40 112.0(4) . . ? O2 V9 O12 109.6(4) . . ? O40 V9 O12 82.0(3) . . ? O2 V9 O13 110.8(4) . . ? O40 V9 O13 136.8(3) . . ? O12 V9 O13 78.5(3) . . ? O2 V9 O15 107.7(4) . . ? O40 V9 O15 78.5(3) . . ? O12 V9 O15 142.1(3) . . ? O13 V9 O15 94.1(3) . . ? O2 V9 V1 109.6(3) . . ? O40 V9 V1 41.2(2) . . ? O12 V9 V1 42.2(2) . . ? O13 V9 V1 116.4(2) . . ? O15 V9 V1 117.2(2) . . ? O2 V9 V10 114.9(3) . . ? O40 V9 V10 112.4(2) . . ? O12 V9 V10 37.9(3) . . ? O13 V9 V10 40.7(2) . . ? O15 V9 V10 125.9(2) . . ? V1 V9 V10 78.12(7) . . ? O2 V9 V7 114.5(4) . . ? O40 V9 V7 36.5(2) . . ? O12 V9 V7 113.4(2) . . ? O13 V9 V7 124.0(3) . . ? O15 V9 V7 42.0(2) . . ? V1 V9 V7 76.65(7) . . ? V10 V9 V7 129.57(8) . . ? O4 V10 O12 112.9(4) . . ? O4 V10 O30 112.4(4) . . ? O12 V10 O30 134.7(3) . . ? O4 V10 O45 103.1(4) . . ? O12 V10 O45 90.7(3) . . ? O30 V10 O45 79.9(3) . . ? O4 V10 O13 106.0(4) . . ? O12 V10 O13 78.4(3) . . ? O30 V10 O13 88.7(3) . . ? O45 V10 O13 151.0(3) . . ? O4 V10 V13 111.2(3) . . ? O12 V10 V13 120.8(2) . . ? O30 V10 V13 38.3(2) . . ? O45 V10 V13 41.7(2) . . ? O13 V10 V13 123.5(2) . . ? O4 V10 V9 113.8(3) . . ? O12 V10 V9 38.3(2) . . ? O30 V10 V9 117.9(2) . . ? O45 V10 V9 125.1(2) . . ? O13 V10 V9 40.2(2) . . ? V13 V10 V9 134.96(8) . . ? O14 V11 O34 110.4(4) . . ? O14 V11 O1 112.6(4) . . ? O34 V11 O1 83.5(3) . . ? O14 V11 O22 109.0(4) . . ? O34 V11 O22 78.2(3) . . ? O1 V11 O22 138.1(3) . . ? O14 V11 O5 110.9(4) . . ? O34 V11 O5 138.6(3) . . ? O1 V11 O5 79.1(3) . . ? O22 V11 O5 90.4(3) . . ? O14 V11 V7 111.5(3) . . ? O34 V11 V7 42.3(2) . . ? O1 V11 V7 42.4(2) . . ? O22 V11 V7 116.1(2) . . ? O5 V11 V7 117.1(2) . . ? O14 V11 V2 116.7(3) . . ? O34 V11 V2 114.7(2) . . ? O1 V11 V2 38.2(2) . . ? O22 V11 V2 121.6(2) . . ? O5 V11 V2 41.0(2) . . ? V7 V11 V2 78.77(7) . . ? O14 V11 V3 113.6(3) . . ? O34 V11 V3 37.8(2) . . ? O1 V11 V3 114.4(2) . . ? O22 V11 V3 40.5(2) . . ? O5 V11 V3 121.7(2) . . ? V7 V11 V3 78.23(7) . . ? V2 V11 V3 129.40(8) . . ? O24 V12 O39 107.1(4) . . ? O24 V12 O46 107.2(4) . . ? O39 V12 O46 90.0(3) . . ? O24 V12 O36 110.0(4) . . ? O39 V12 O36 82.4(3) . . ? O46 V12 O36 142.7(3) . . ? O24 V12 O41 105.9(4) . . ? O39 V12 O41 146.8(3) . . ? O46 V12 O41 76.9(3) . . ? O36 V12 O41 89.7(3) . . ? O24 V12 V4 108.4(3) . . ? O39 V12 V4 41.1(2) . . ? O46 V12 V4 126.0(2) . . ? O36 V12 V4 42.1(2) . . ? O41 V12 V4 128.0(2) . . ? O24 V12 V13 109.4(3) . . ? O39 V12 V13 122.5(2) . . ? O46 V12 V13 37.3(2) . . ? O36 V12 V13 122.5(2) . . ? O41 V12 V13 39.7(2) . . ? V4 V12 V13 142.09(8) . . ? O25 V13 O30 111.5(4) . . ? O25 V13 O46 110.3(4) . . ? O30 V13 O46 82.8(3) . . ? O25 V13 O41 108.5(4) . . ? O30 V13 O41 139.6(3) . . ? O46 V13 O41 78.5(3) . . ? O25 V13 O45 110.7(4) . . ? O30 V13 O45 79.6(3) . . ? O46 V13 O45 138.9(3) . . ? O41 V13 O45 91.5(3) . . ? O25 V13 V5 110.6(3) . . ? O30 V13 V5 42.8(2) . . ? O46 V13 V5 41.2(2) . . ? O41 V13 V5 116.0(2) . . ? O45 V13 V5 118.0(2) . . ? O25 V13 V10 115.6(3) . . ? O30 V13 V10 39.1(2) . . ? O46 V13 V10 115.1(2) . . ? O41 V13 V10 123.1(2) . . ? O45 V13 V10 40.6(2) . . ? V5 V13 V10 80.07(7) . . ? O25 V13 V12 113.4(3) . . ? O30 V13 V12 114.4(2) . . ? O46 V13 V12 37.9(2) . . ? O41 V13 V12 40.7(2) . . ? O45 V13 V12 122.7(2) . . ? V5 V13 V12 77.54(7) . . ? V10 V13 V12 130.55(8) . . ? O17 V14 O39 108.3(4) . . ? O17 V14 O44 109.0(4) . . ? O39 V14 O44 89.8(3) . . ? O17 V14 O28 108.1(4) . . ? O39 V14 O28 143.3(3) . . ? O44 V14 O28 83.1(3) . . ? O17 V14 O38 103.9(4) . . ? O39 V14 O38 77.6(3) . . ? O44 V14 O38 147.0(3) . . ? O28 V14 O38 89.0(3) . . ? O17 V14 V15 107.9(3) . . ? O39 V14 V15 127.0(2) . . ? O44 V14 V15 41.9(2) . . ? O28 V14 V15 42.3(2) . . ? O38 V14 V15 127.9(2) . . ? O17 V14 V4 108.6(3) . . ? O39 V14 V4 37.2(2) . . ? O44 V14 V4 122.4(2) . . ? O28 V14 V4 123.0(2) . . ? O38 V14 V4 40.5(2) . . ? V15 V14 V4 143.47(8) . . ? O43 V15 O44 110.2(4) . . ? O43 V15 O28 112.2(4) . . ? O44 V15 O28 83.9(3) . . ? O43 V15 O47 112.7(4) . . ? O44 V15 O47 137.0(3) . . ? O28 V15 O47 79.1(3) . . ? O43 V15 O18 108.2(4) . . ? O44 V15 O18 77.3(3) . . ? O28 V15 O18 139.2(3) . . ? O47 V15 O18 90.5(3) . . ? O43 V15 V14 111.7(3) . . ? O44 V15 V14 42.4(2) . . ? O28 V15 V14 42.5(2) . . ? O47 V15 V14 116.3(2) . . ? O18 V15 V14 115.6(2) . . ? O43 V15 V2 117.0(3) . . ? O44 V15 V2 115.0(2) . . ? O28 V15 V2 38.6(2) . . ? O47 V15 V2 40.7(2) . . ? O18 V15 V2 122.5(2) . . ? V14 V15 V2 78.90(7) . . ? O43 V15 V5 113.4(3) . . ? O44 V15 V5 37.0(2) . . ? O28 V15 V5 114.3(2) . . ? O47 V15 V5 120.5(2) . . ? O18 V15 V5 40.3(2) . . ? V14 V15 V5 77.53(7) . . ? V2 V15 V5 129.20(8) . . ? V2 O1 V11 103.1(4) . . ? V2 O1 V7 151.0(4) . . ? V11 O1 V7 95.3(3) . . ? Ge6 O5 V11 135.3(4) . . ? Ge6 O5 V2 125.0(4) . . ? V11 O5 V2 98.1(3) . . ? Ge4 O7 V8 131.2(4) . . ? Ge4 O7 V1 128.1(4) . . ? V8 O7 V1 97.5(3) . . ? Ge6 O11 Mn3 130.9(5) . . ? V10 O12 V9 103.8(3) . . ? V10 O12 V1 149.3(4) . . ? V9 O12 V1 96.2(4) . . ? Ge5 O13 V9 132.5(4) . . ? Ge5 O13 V10 125.7(4) . . ? V9 O13 V10 99.1(3) . . ? Ge2 O15 V9 132.7(5) . . ? Ge2 O15 V7 127.4(4) . . ? V9 O15 V7 96.3(3) . . ? Ge5 O18 V5 127.0(4) . . ? Ge5 O18 V15 132.7(4) . . ? V5 O18 V15 99.0(3) . . ? Ge3 O19 Mn4 127.5(4) . . ? Ge4 O20 Ge3 119.1(4) . . ? Ge1 O22 V11 134.1(4) . . ? Ge1 O22 V3 125.7(4) . . ? V11 O22 V3 99.6(4) . . ? V6 O26 V8 103.4(4) . . ? V6 O26 V3 152.0(5) . . ? V8 O26 V3 95.3(3) . . ? Ge3 O27 V6 124.9(4) . . ? Ge3 O27 V8 134.7(5) . . ? V6 O27 V8 99.2(3) . . ? V15 O28 V2 102.9(3) . . ? V15 O28 V14 95.2(3) . . ? V2 O28 V14 149.7(4) . . ? Ge1 O29 Ge6 116.5(4) . . ? V13 O30 V5 94.9(3) . . ? V13 O30 V10 102.7(3) . . ? V5 O30 V10 151.9(4) . . ? Ge5 O31 Ge2 118.8(4) . . ? V5 O32 Mn5 150.9(5) . . ? V11 O34 V3 105.4(4) . . ? V11 O34 V7 96.6(4) . . ? V3 O34 V7 148.8(4) . . ? V1 O35 V8 106.3(4) . . ? V1 O35 V3 150.0(4) . . ? V8 O35 V3 96.7(3) . . ? V4 O36 V12 95.4(4) . . ? V4 O36 V6 102.6(4) . . ? V12 O36 V6 148.7(4) . . ? Ge2 O37 Mn1 135.1(4) . 3_755 ? Ge2 O37 Mn2 132.9(4) . 3_755 ? Mn1 O37 Mn2 91.0(3) 3_755 3_755 ? Ge6 O38 V4 135.1(4) . . ? Ge6 O38 V14 125.5(4) . . ? V4 O38 V14 98.8(3) . . ? V12 O39 V4 98.0(3) . . ? V12 O39 V14 147.8(4) . . ? V4 O39 V14 104.9(4) . . ? V9 O40 V7 107.7(4) . . ? V9 O40 V1 99.0(4) . . ? V7 O40 V1 148.5(4) . . ? Ge3 O41 V13 134.5(4) . . ? Ge3 O41 V12 124.9(4) . . ? V13 O41 V12 99.7(3) . . ? Ge4 O42 Mn2 132.5(4) . . ? Ge4 O42 Mn1 125.6(4) . . ? Mn2 O42 Mn1 93.0(3) . . ? V5 O44 V15 105.6(4) . . ? V5 O44 V14 148.9(4) . . ? V15 O44 V14 95.7(3) . . ? Ge4 O45 V10 126.2(4) . . ? Ge4 O45 V13 134.6(4) . . ? V10 O45 V13 97.7(3) . . ? V5 O46 V13 96.7(3) . . ? V5 O46 V12 150.1(4) . . ? V13 O46 V12 104.8(3) . . ? Ge2 O47 V15 135.6(4) . . ? Ge2 O47 V2 125.3(4) . . ? V15 O47 V2 98.7(3) . . ? Ge1 O48 V6 126.2(4) . . ? Ge1 O48 V4 131.8(4) . . ? V6 O48 V4 98.2(3) . . ? O37 Mn1 O42 81.9(3) 3_745 . ? O37 Mn1 N12 93.7(4) 3_745 . ? O42 Mn1 N12 157.5(4) . . ? O37 Mn1 N14 91.8(4) 3_745 . ? O42 Mn1 N14 101.8(3) . . ? N12 Mn1 N14 100.4(4) . . ? O37 Mn1 N11 165.9(4) 3_745 . ? O42 Mn1 N11 109.8(4) . . ? N12 Mn1 N11 78.5(4) . . ? N14 Mn1 N11 78.3(4) . . ? O37 Mn1 N13 118.9(4) 3_745 . ? O42 Mn1 N13 74.6(4) . . ? N12 Mn1 N13 88.7(4) . . ? N14 Mn1 N13 147.5(5) . . ? N11 Mn1 N13 73.0(5) . . ? O37 Mn1 Mn2 46.9(2) 3_745 . ? O42 Mn1 Mn2 42.8(2) . . ? N12 Mn1 Mn2 120.6(3) . . ? N14 Mn1 Mn2 119.4(3) . . ? N11 Mn1 Mn2 147.1(3) . . ? N13 Mn1 Mn2 80.4(3) . . ? O42 Mn2 N24 96.9(4) . . ? O42 Mn2 N22 120.0(4) . . ? N24 Mn2 N22 138.6(4) . . ? O42 Mn2 O37 78.9(3) . 3_745 ? N24 Mn2 O37 90.3(3) . 3_745 ? N22 Mn2 O37 80.1(3) . 3_745 ? O42 Mn2 N23 87.4(4) . . ? N24 Mn2 N23 112.5(4) . . ? N22 Mn2 N23 88.8(4) . . ? O37 Mn2 N23 154.7(4) 3_745 . ? O42 Mn2 N21 156.9(4) . . ? N24 Mn2 N21 76.9(4) . . ? N22 Mn2 N21 75.1(4) . . ? O37 Mn2 N21 122.9(4) 3_745 . ? N23 Mn2 N21 74.9(4) . . ? O42 Mn2 Mn1 44.2(2) . . ? N24 Mn2 Mn1 113.7(3) . . ? N22 Mn2 Mn1 85.4(3) . . ? O37 Mn2 Mn1 42.1(2) 3_745 . ? N23 Mn2 Mn1 114.9(3) . . ? N21 Mn2 Mn1 158.2(3) . . ? O11 Mn3 N32 103.3(4) . . ? O11 Mn3 N33 104.6(4) . . ? N32 Mn3 N33 111.6(4) . . ? O11 Mn3 N34 99.9(5) . . ? N32 Mn3 N34 107.1(5) . . ? N33 Mn3 N34 127.2(5) . . ? O11 Mn3 N31 178.7(4) . . ? N32 Mn3 N31 76.6(5) . . ? N33 Mn3 N31 76.7(4) . . ? N34 Mn3 N31 78.9(5) . . ? O19 Mn4 N44 101.6(5) . . ? O19 Mn4 N42 99.7(5) . . ? N44 Mn4 N42 113.9(5) . . ? O19 Mn4 N43 104.0(4) . . ? N44 Mn4 N43 110.9(6) . . ? N42 Mn4 N43 123.0(6) . . ? O19 Mn4 N41 177.6(5) . . ? N44 Mn4 N41 79.4(6) . . ? N42 Mn4 N41 77.9(6) . . ? N43 Mn4 N41 77.7(5) . . ? N62 Mn5 N52 98.2(6) . . ? N62 Mn5 N53 105.7(7) . . ? N52 Mn5 N53 98.4(6) . . ? N62 Mn5 O32 86.4(5) . . ? N52 Mn5 O32 172.6(5) . . ? N53 Mn5 O32 85.9(4) . . ? N62 Mn5 N54 101.3(7) . . ? N52 Mn5 N54 93.8(6) . . ? N53 Mn5 N54 148.3(7) . . ? O32 Mn5 N54 79.5(5) . . ? N62 Mn5 N51 176.0(6) . . ? N52 Mn5 N51 78.0(5) . . ? N53 Mn5 N51 76.3(6) . . ? O32 Mn5 N51 97.3(4) . . ? N54 Mn5 N51 77.8(6) . . ? C11 N11 C13 113.8(16) . . ? C11 N11 C15 109.0(16) . . ? C13 N11 C15 111.9(14) . . ? C11 N11 Mn1 109.4(10) . . ? C13 N11 Mn1 106.7(11) . . ? C15 N11 Mn1 105.8(9) . . ? C12 N12 Mn1 108.2(8) . . ? C14 N13 Mn1 110.3(11) . . ? C16 N14 Mn1 110.5(9) . . ? C12 C11 N11 112.1(17) . . ? C11 C12 N12 110.2(14) . . ? C14 C13 N11 116.6(17) . . ? C13 C14 N13 109.7(15) . . ? C16 C15 N11 110.6(13) . . ? C15 C16 N14 111.9(13) . . ? C25 N21 C23 113.0(14) . . ? C25 N21 C21 111.1(14) . . ? C23 N21 C21 107.8(12) . . ? C25 N21 Mn2 106.7(10) . . ? C23 N21 Mn2 107.0(9) . . ? C21 N21 Mn2 111.2(9) . . ? C22 N22 Mn2 105.1(9) . . ? C24 N23 Mn2 111.7(8) . . ? C26 N24 Mn2 112.4(9) . . ? N21 C21 C22 110.2(12) . . ? C21 C22 N22 109.9(11) . . ? C24 C23 N21 113.5(12) . . ? C23 C24 N23 113.9(11) . . ? N21 C25 C26 113.3(15) . . ? N24 C26 C25 110.9(14) . . ? C33 N31 C36 107.5(15) . . ? C33 N31 C31 115.7(13) . . ? C36 N31 C31 116.4(13) . . ? C33 N31 Mn3 106.8(9) . . ? C36 N31 Mn3 103.3(11) . . ? C31 N31 Mn3 106.0(10) . . ? C32 N32 Mn3 114.0(9) . . ? C34 N33 Mn3 111.9(8) . . ? C35 N34 Mn3 108.0(10) . . ? N31 C31 C32 112.5(13) . . ? N32 C32 C31 108.3(13) . . ? N31 C33 C34 115.9(13) . . ? N33 C34 C33 112.3(13) . . ? C36 C35 N34 113.6(15) . . ? N31 C36 C35 112.6(18) . . ? C43 N41 C45 114.5(15) . . ? C43 N41 C41 113.8(17) . . ? C45 N41 C41 110.1(15) . . ? C43 N41 Mn4 104.5(10) . . ? C45 N41 Mn4 108.5(12) . . ? C41 N41 Mn4 104.6(11) . . ? C42 N42 Mn4 113.4(11) . . ? C44 N43 Mn4 113.5(10) . . ? C46 N44 Mn4 109.9(14) . . ? C42 C41 N41 118.2(17) . . ? C41 C42 N42 105.8(19) . . ? N41 C43 C44 116.0(16) . . ? N43 C44 C43 108.8(14) . . ? N41 C45 C46 111.1(16) . . ? C45 C46 N44 113.8(16) . . ? C53 N51 C51 114.0(17) . . ? C53 N51 C55 110.3(16) . . ? C51 N51 C55 113.1(16) . . ? C53 N51 Mn5 105.4(12) . . ? C51 N51 Mn5 109.0(10) . . ? C55 N51 Mn5 104.4(11) . . ? C52 N52 Mn5 110.0(10) . . ? C54 N53 Mn5 112.9(12) . . ? C56 N54 Mn5 111.0(14) . . ? N51 C51 C52 116.1(14) . . ? N52 C52 C51 111.1(15) . . ? N51 C53 C54 114.3(17) . . ? N53 C54 C53 110.6(18) . . ? N51 C55 C56 109.5(18) . . ? N54 C56 C55 109.4(17) . . ? C61 N61 C65 117(3) . . ? C61 N61 C63 112(2) . . ? C65 N61 C63 110(3) . . ? C62 N62 Mn5 113.6(13) . . ? C62 C61 N61 118(2) . . ? C61 C62 N62 112(2) . . ? C64 C63 N61 108(3) . . ? C63 C64 N63 115(3) . . ? C66 C65 N61 106(3) . . ? N64 C66 C65 123(3) . . ? # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.011 0.250 0.000 722.7 392.5 2 -0.096 -0.250 0.500 722.8 424.4 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 24.76 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.833 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.120 _database_code_depnum_ccdc_archive 'CCDC 905606' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Jwang425 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H118 Ge6 N24 Ni4 O51 V15' _chemical_formula_weight 3138.02 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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.9906(4) _cell_length_b 14.7778(3) _cell_length_c 24.9887(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.5730(10) _cell_angle_gamma 90.00 _cell_volume 9963.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10614 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 26.0 _exptl_crystal_description polyhedra _exptl_crystal_colour black _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.092 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6236 _exptl_absorpt_coefficient_mu 3.941 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.621 _exptl_absorpt_correction_T_max 0.782 _exptl_absorpt_process_details 'X-Shape (STOE & CIE, 1998)' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68940 _diffrn_reflns_av_R_equivalents 0.0699 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9771 _reflns_number_gt 9027 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE-IPDS Program Package' _computing_cell_refinement 'STOE-IPDS Program Package' _computing_data_reduction 'STOE-IPDS Program Package' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+86.2935P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00025(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9771 _refine_ls_number_parameters 625 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1425 _refine_ls_wR_factor_gt 0.1387 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1 Ge 0.37868(2) 0.51136(4) 0.25295(3) 0.03535(16) Uani 1 1 d . . . Ge2 Ge 0.55091(2) 1.02739(4) 0.22858(2) 0.03399(16) Uani 1 1 d . . . Ge3 Ge 0.65049(2) 0.65864(4) 0.32585(2) 0.03368(16) Uani 1 1 d . . . Ni1 Ni 0.73974(4) 0.28910(6) 0.33488(3) 0.0455(2) Uani 1 1 d . . . Ni2 Ni 0.56011(3) 0.70538(6) 0.53178(3) 0.0435(2) Uani 1 1 d . . . V1 V 0.36594(4) 0.72834(7) 0.30403(4) 0.0345(2) Uani 1 1 d . . . V2 V 0.43151(4) 0.85498(6) 0.35666(4) 0.0330(2) Uani 1 1 d . . . V3 V 0.53913(4) 0.92630(6) 0.35233(4) 0.0332(2) Uani 1 1 d . . . V4 V 0.62374(4) 0.86828(6) 0.28353(4) 0.0329(2) Uani 1 1 d . . . V5 V 0.55236(4) 0.74546(6) 0.38820(4) 0.0306(2) Uani 1 1 d . . . V6 V 0.54329(4) 0.54671(6) 0.35349(4) 0.0339(2) Uani 1 1 d . . . V7 V 0.44079(4) 0.60278(6) 0.35861(4) 0.0331(2) Uani 1 1 d . . . V8 V 0.5000 0.47001(9) 0.2500 0.0327(3) Uani 1 2 d S . . O1 O 0.38814(16) 0.6000(3) 0.29929(17) 0.0380(9) Uani 1 1 d . . . O2 O 0.64632(16) 0.7393(3) 0.27479(16) 0.0366(9) Uani 1 1 d . . . O3 O 0.61061(16) 0.8496(3) 0.20795(17) 0.0380(9) Uani 1 1 d . . . O4 O 0.41706(16) 0.7262(3) 0.35726(17) 0.0386(9) Uani 1 1 d . . . O5 O 0.31190(17) 0.7331(3) 0.33069(18) 0.0444(10) Uani 1 1 d . . . O6 O 0.52976(16) 0.9572(3) 0.17674(16) 0.0366(9) Uani 1 1 d . . . O7 O 0.49937(16) 0.8301(3) 0.37889(16) 0.0371(9) Uani 1 1 d . . . O8 O 0.40060(18) 0.8973(3) 0.40451(18) 0.0470(11) Uani 1 1 d . . . O9 O 0.57040(16) 0.9621(3) 0.28362(17) 0.0378(9) Uani 1 1 d . . . O10 O 0.58876(16) 0.8328(3) 0.34628(16) 0.0363(9) Uani 1 1 d . . . O11 O 0.55621(19) 0.9949(3) 0.39907(18) 0.0471(11) Uani 1 1 d . . . O12 O 0.67505(18) 0.9208(3) 0.2949(2) 0.0478(11) Uani 1 1 d . . . O13 O 0.56948(17) 0.7507(3) 0.45062(16) 0.0375(9) Uani 1 1 d . . . O14 O 0.59379(16) 0.6459(3) 0.35618(16) 0.0375(9) Uani 1 1 d . . . O15 O 0.50627(16) 0.6453(3) 0.38157(16) 0.0360(9) Uani 1 1 d . . . O16 O 0.51967(16) 0.5165(3) 0.18169(17) 0.0375(9) Uani 1 1 d . . . O17 O 0.43438(16) 0.5030(3) 0.21755(16) 0.0387(9) Uani 1 1 d . . . O18 O 0.5577(2) 0.4762(3) 0.4008(2) 0.0517(12) Uani 1 1 d . . . O19 O 0.41760(18) 0.5510(3) 0.40874(17) 0.0454(10) Uani 1 1 d . . . O20 O 0.5000 0.3607(4) 0.2500 0.0397(13) Uani 1 2 d S . . O21 O 0.35736(18) 0.4120(3) 0.27696(19) 0.0463(11) Uani 1 1 d . . . O22 O 0.5000 1.0913(4) 0.2500 0.0390(13) Uani 1 2 d S . . O23 O 0.59774(18) 1.0968(3) 0.20650(19) 0.0467(11) Uani 1 1 d . . . O24 O 0.69788(18) 0.6884(3) 0.37038(19) 0.0459(11) Uani 1 1 d . . . O25 O 0.66479(16) 0.5545(3) 0.29568(17) 0.0384(9) Uani 1 1 d . . . O26 O 0.5000 0.7302(14) 0.2500 0.174(7) Uani 1 2 d S . . O27 O 0.4120(2) 0.2694(4) 0.2705(4) 0.087(2) Uani 1 1 d . . . N1 N 0.7084(2) 0.1614(5) 0.3262(3) 0.0566(15) Uani 1 1 d . A . N2 N 0.7365(2) 0.2903(4) 0.2506(2) 0.0504(14) Uani 1 1 d . A . H1N H 0.7188 0.3384 0.2389 0.061 Uiso 1 1 calc R . . H2N H 0.7673 0.2947 0.2379 0.061 Uiso 1 1 calc R . . N3 N 0.7456(3) 0.2480(5) 0.4167(3) 0.0660(18) Uani 1 1 d . A . H3N H 0.7771 0.2547 0.4289 0.079 Uiso 1 1 calc R . . H4N H 0.7260 0.2831 0.4367 0.079 Uiso 1 1 calc R . . N4 N 0.6662(3) 0.3309(6) 0.3377(3) 0.082(2) Uani 1 1 d . A . H5N H 0.6635 0.3793 0.3593 0.098 Uiso 1 1 calc R . . H6N H 0.6547 0.3461 0.3048 0.098 Uiso 1 1 calc R . . C1 C 0.7221(3) 0.1305(5) 0.2722(3) 0.0590(19) Uani 1 1 d . . . H1A H 0.7027 0.0776 0.2622 0.071 Uiso 1 1 calc R A . H1B H 0.7568 0.1136 0.2726 0.071 Uiso 1 1 calc R . . C2 C 0.7128(3) 0.2054(5) 0.2312(3) 0.0559(18) Uani 1 1 d . A . H2A H 0.7264 0.1882 0.1972 0.067 Uiso 1 1 calc R . . H2B H 0.6774 0.2148 0.2259 0.067 Uiso 1 1 calc R . . C3 C 0.7323(4) 0.1049(6) 0.3689(4) 0.073(2) Uani 1 1 d . . . H3A H 0.7665 0.0933 0.3602 0.087 Uiso 1 1 calc R A . H3B H 0.7153 0.0472 0.3709 0.087 Uiso 1 1 calc R . . C4 C 0.7304(4) 0.1521(7) 0.4217(4) 0.083(3) Uani 1 1 d . A . H4A H 0.6970 0.1492 0.4349 0.100 Uiso 1 1 calc R . . H4B H 0.7523 0.1218 0.4474 0.100 Uiso 1 1 calc R . . C5 C 0.6539(3) 0.1675(9) 0.3315(4) 0.084(3) Uani 1 1 d . . . H5A H 0.6426 0.1163 0.3521 0.101 Uiso 1 1 calc R A . H5B H 0.6382 0.1641 0.2962 0.101 Uiso 1 1 calc R . . C6 C 0.6379(4) 0.2545(10) 0.3585(4) 0.098(4) Uani 1 1 d . A . H6A H 0.6028 0.2644 0.3518 0.117 Uiso 1 1 calc R . . H6B H 0.6437 0.2497 0.3969 0.117 Uiso 1 1 calc R . . N11 N 0.5173(2) 0.8181(4) 0.5500(2) 0.0482(13) Uani 1 1 d . . . N12 N 0.6197(2) 0.7916(4) 0.5492(3) 0.0536(15) Uani 1 1 d . . . H11N H 0.6392 0.7673 0.5753 0.064 Uiso 1 1 calc R . . H12N H 0.6380 0.7989 0.5200 0.064 Uiso 1 1 calc R . . N13 N 0.4906(2) 0.6537(5) 0.5044(2) 0.0559(16) Uani 1 1 d . . . H13N H 0.4930 0.6338 0.4705 0.067 Uiso 1 1 calc R . . H14N H 0.4819 0.6067 0.5250 0.067 Uiso 1 1 calc R . . N14 N 0.5479(3) 0.6689(4) 0.6116(3) 0.0568(16) Uani 1 1 d . . . H15N H 0.5448 0.6085 0.6146 0.068 Uiso 1 1 calc R . . H16N H 0.5732 0.6873 0.6330 0.068 Uiso 1 1 calc R . . C11 C 0.5507(4) 0.8986(5) 0.5415(3) 0.062(2) Uani 1 1 d . . . H11A H 0.5542 0.9091 0.5035 0.075 Uiso 1 1 calc R . . H11B H 0.5361 0.9522 0.5570 0.075 Uiso 1 1 calc R . . C12 C 0.6002(4) 0.8815(6) 0.5671(4) 0.068(2) Uani 1 1 d . . . H12A H 0.5976 0.8819 0.6057 0.082 Uiso 1 1 calc R . . H12B H 0.6230 0.9291 0.5573 0.082 Uiso 1 1 calc R . . C13 C 0.4757(3) 0.8190(6) 0.5120(3) 0.064(2) Uani 1 1 d . . . H13A H 0.4868 0.8393 0.4774 0.076 Uiso 1 1 calc R . . H13B H 0.4508 0.8612 0.5240 0.076 Uiso 1 1 calc R . . C14 C 0.4528(3) 0.7242(7) 0.5065(4) 0.068(2) Uani 1 1 d . . . H14A H 0.4319 0.7129 0.5367 0.082 Uiso 1 1 calc R . . H14B H 0.4322 0.7217 0.4742 0.082 Uiso 1 1 calc R . . C15 C 0.5018(3) 0.8115(5) 0.6067(3) 0.0554(18) Uani 1 1 d . . . H15A H 0.4690 0.8375 0.6097 0.067 Uiso 1 1 calc R . . H15B H 0.5245 0.8465 0.6293 0.067 Uiso 1 1 calc R . . C16 C 0.5011(3) 0.7150(5) 0.6263(3) 0.0581(19) Uani 1 1 d . . . H16A H 0.4979 0.7140 0.6648 0.070 Uiso 1 1 calc R . . H16B H 0.4729 0.6834 0.6102 0.070 Uiso 1 1 calc R . . N21 N 0.7248(2) 0.5567(4) 0.4446(2) 0.0522(14) Uani 1 1 d . . . N22 N 0.7857(4) 0.4108(7) 0.3432(4) 0.050(2) Uani 0.65 1 d P A 1 H21N H 0.8141 0.3934 0.3599 0.060 Uiso 0.65 1 calc PR A 1 H22N H 0.7937 0.4273 0.3099 0.060 Uiso 0.65 1 calc PR A 1 N22' N 0.7587(8) 0.4266(14) 0.3300(9) 0.059(5) Uani 0.35 1 d P A 2 H23N H 0.7847 0.4277 0.3083 0.071 Uiso 0.35 1 calc PR A 2 H24N H 0.7334 0.4517 0.3111 0.071 Uiso 0.35 1 calc PR A 2 N23 N 0.6007(3) 0.5916(4) 0.5093(3) 0.0563(15) Uani 1 1 d . . . H25N H 0.6024 0.5527 0.5370 0.068 Uiso 1 1 calc R . . H26N H 0.5846 0.5638 0.4820 0.068 Uiso 1 1 calc R . . N24 N 0.8199(4) 0.6421(6) 0.5491(4) 0.089(3) Uani 1 1 d . . . C21 C 0.7476(4) 0.4754(6) 0.4211(4) 0.068(2) Uani 1 1 d . A . H21A H 0.7727 0.4526 0.4461 0.081 Uiso 1 1 calc R . . H21B H 0.7223 0.4291 0.4169 0.081 Uiso 1 1 calc R . . C22 C 0.7704(4) 0.4903(7) 0.3692(4) 0.074(3) Uani 1 1 d . . . H22A H 0.7468 0.5217 0.3459 0.089 Uiso 0.65 1 calc PR A 1 H22B H 0.7989 0.5295 0.3745 0.089 Uiso 0.65 1 calc PR A 1 H22C H 0.7604 0.5495 0.3560 0.089 Uiso 0.35 1 calc PR A 2 H22D H 0.8061 0.4912 0.3747 0.089 Uiso 0.35 1 calc PR A 2 C23 C 0.6791(3) 0.5324(5) 0.4726(3) 0.0577(19) Uani 1 1 d . . . H23A H 0.6877 0.4931 0.5025 0.069 Uiso 1 1 calc R . . H23B H 0.6574 0.4988 0.4483 0.069 Uiso 1 1 calc R . . C24 C 0.6516(3) 0.6138(5) 0.4930(3) 0.0559(18) Uani 1 1 d . . . H24A H 0.6700 0.6390 0.5234 0.067 Uiso 1 1 calc R . . H24B H 0.6500 0.6595 0.4652 0.067 Uiso 1 1 calc R . . C25 C 0.7611(3) 0.6147(6) 0.4750(3) 0.0601(19) Uani 1 1 d . . . H25A H 0.7448 0.6713 0.4832 0.072 Uiso 1 1 calc R . . H25B H 0.7881 0.6287 0.4516 0.072 Uiso 1 1 calc R . . C26 C 0.7831(4) 0.5775(7) 0.5261(4) 0.082(3) Uani 1 1 d . . . H26A H 0.7570 0.5673 0.5514 0.098 Uiso 1 1 calc R . . H26B H 0.7990 0.5200 0.5192 0.098 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.0401(3) 0.0287(3) 0.0370(3) 0.0015(2) -0.0032(3) -0.0036(2) Ge2 0.0430(4) 0.0255(3) 0.0334(3) 0.0008(2) 0.0002(3) -0.0032(2) Ge3 0.0364(3) 0.0305(3) 0.0339(3) 0.0000(2) -0.0027(2) 0.0001(2) Ni1 0.0538(5) 0.0414(4) 0.0414(4) 0.0006(3) 0.0035(4) 0.0068(4) Ni2 0.0552(5) 0.0397(4) 0.0357(4) 0.0008(3) 0.0045(4) 0.0033(4) V1 0.0367(5) 0.0330(5) 0.0338(5) 0.0017(4) 0.0012(4) -0.0014(4) V2 0.0392(5) 0.0288(5) 0.0311(5) -0.0013(4) 0.0013(4) 0.0025(4) V3 0.0413(5) 0.0273(5) 0.0309(5) -0.0024(4) 0.0001(4) 0.0005(4) V4 0.0374(5) 0.0281(5) 0.0333(5) 0.0002(4) 0.0008(4) -0.0020(4) V5 0.0373(5) 0.0275(4) 0.0268(4) 0.0001(3) -0.0006(4) -0.0004(4) V6 0.0426(5) 0.0271(5) 0.0319(5) 0.0015(4) -0.0033(4) -0.0015(4) V7 0.0402(5) 0.0282(5) 0.0308(5) 0.0027(4) 0.0000(4) -0.0031(4) V8 0.0410(8) 0.0253(6) 0.0316(7) 0.000 -0.0032(6) 0.000 O1 0.042(2) 0.033(2) 0.038(2) 0.0006(17) -0.0049(18) 0.0008(18) O2 0.043(2) 0.032(2) 0.034(2) 0.0007(16) -0.0030(17) 0.0022(17) O3 0.045(2) 0.029(2) 0.040(2) 0.0018(17) 0.0033(18) -0.0016(17) O4 0.044(2) 0.033(2) 0.039(2) 0.0006(17) -0.0023(18) -0.0007(18) O5 0.037(2) 0.052(3) 0.044(2) 0.003(2) 0.0027(19) -0.004(2) O6 0.044(2) 0.029(2) 0.037(2) -0.0031(16) -0.0021(18) -0.0024(17) O7 0.040(2) 0.033(2) 0.038(2) 0.0017(17) 0.0029(17) 0.0004(17) O8 0.054(3) 0.046(3) 0.042(2) -0.006(2) 0.009(2) 0.008(2) O9 0.045(2) 0.029(2) 0.040(2) 0.0024(17) 0.0038(18) 0.0034(17) O10 0.043(2) 0.030(2) 0.036(2) -0.0011(16) 0.0017(17) -0.0008(17) O11 0.061(3) 0.039(2) 0.041(2) -0.0101(19) -0.003(2) 0.002(2) O12 0.046(3) 0.039(2) 0.058(3) -0.001(2) -0.001(2) -0.010(2) O13 0.051(2) 0.035(2) 0.0271(19) 0.0004(16) -0.0003(17) 0.0023(18) O14 0.043(2) 0.031(2) 0.038(2) -0.0015(17) 0.0008(18) -0.0028(17) O15 0.041(2) 0.032(2) 0.034(2) -0.0020(16) -0.0005(17) -0.0001(17) O16 0.041(2) 0.031(2) 0.040(2) 0.0012(17) -0.0033(18) 0.0006(17) O17 0.043(2) 0.038(2) 0.036(2) 0.0005(17) -0.0046(18) -0.0006(18) O18 0.070(3) 0.034(2) 0.050(3) 0.011(2) -0.016(2) -0.004(2) O19 0.055(3) 0.043(2) 0.038(2) 0.0092(19) 0.003(2) -0.008(2) O20 0.052(4) 0.029(3) 0.039(3) 0.000 -0.002(3) 0.000 O21 0.051(3) 0.032(2) 0.056(3) 0.003(2) 0.003(2) -0.006(2) O22 0.050(4) 0.025(3) 0.042(3) 0.000 -0.002(3) 0.000 O23 0.051(3) 0.039(2) 0.050(3) 0.000(2) 0.006(2) -0.011(2) O24 0.048(3) 0.042(2) 0.047(3) -0.003(2) -0.009(2) -0.004(2) O25 0.040(2) 0.034(2) 0.041(2) -0.0010(17) -0.0028(18) 0.0047(18) O26 0.22(2) 0.200(18) 0.104(11) 0.000 0.029(12) 0.000 O27 0.059(4) 0.032(3) 0.169(7) 0.011(3) -0.005(4) -0.005(2) N1 0.055(4) 0.061(4) 0.053(4) 0.005(3) 0.001(3) -0.010(3) N2 0.053(4) 0.051(3) 0.047(3) 0.003(3) -0.001(3) 0.006(3) N3 0.085(5) 0.057(4) 0.056(4) 0.006(3) 0.001(4) -0.003(4) N4 0.073(5) 0.104(6) 0.069(5) -0.013(5) -0.002(4) 0.040(5) C1 0.062(5) 0.055(4) 0.060(5) -0.010(4) 0.004(4) -0.018(4) C2 0.054(4) 0.064(5) 0.050(4) -0.008(3) 0.004(3) -0.007(4) C3 0.098(7) 0.047(4) 0.073(6) 0.016(4) -0.007(5) -0.007(4) C4 0.109(8) 0.069(6) 0.070(6) 0.022(5) -0.016(5) -0.023(6) C5 0.057(5) 0.132(9) 0.063(5) 0.006(6) 0.007(4) -0.028(6) C6 0.056(5) 0.171(13) 0.067(6) -0.010(7) 0.011(5) 0.024(7) N11 0.061(4) 0.042(3) 0.041(3) 0.003(2) 0.007(3) 0.003(3) N12 0.055(4) 0.059(4) 0.047(3) -0.003(3) 0.002(3) -0.005(3) N13 0.066(4) 0.061(4) 0.041(3) -0.005(3) 0.007(3) -0.019(3) N14 0.070(4) 0.047(3) 0.053(4) 0.011(3) 0.007(3) 0.006(3) C11 0.105(7) 0.036(4) 0.046(4) -0.002(3) 0.012(4) -0.013(4) C12 0.080(6) 0.055(5) 0.070(5) -0.021(4) 0.017(4) -0.021(4) C13 0.069(5) 0.072(5) 0.051(4) 0.004(4) 0.010(4) 0.021(4) C14 0.060(5) 0.091(6) 0.054(5) -0.006(4) 0.001(4) -0.001(5) C15 0.072(5) 0.054(4) 0.041(4) -0.001(3) 0.010(3) 0.006(4) C16 0.079(6) 0.053(4) 0.043(4) 0.001(3) 0.012(4) -0.004(4) N21 0.059(4) 0.047(3) 0.051(3) -0.008(3) 0.001(3) 0.005(3) N22 0.050(6) 0.043(5) 0.058(6) -0.008(4) 0.010(5) -0.001(5) N22' 0.048(12) 0.052(12) 0.076(14) 0.005(10) 0.006(11) -0.010(10) N23 0.073(4) 0.044(3) 0.052(3) 0.007(3) 0.007(3) 0.001(3) N24 0.098(7) 0.088(6) 0.081(6) 0.003(5) -0.011(5) -0.026(5) C21 0.081(6) 0.054(5) 0.068(5) -0.012(4) 0.013(5) 0.013(4) C22 0.077(6) 0.071(6) 0.075(6) -0.028(5) 0.010(5) -0.007(5) C23 0.067(5) 0.050(4) 0.057(4) 0.000(3) 0.011(4) 0.005(4) C24 0.063(5) 0.049(4) 0.055(4) 0.001(3) 0.007(4) 0.007(4) C25 0.056(5) 0.062(5) 0.062(5) -0.002(4) 0.001(4) -0.001(4) C26 0.094(7) 0.083(7) 0.068(6) 0.003(5) -0.020(5) -0.015(6) _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 O21 1.693(4) . ? Ge1 O1 1.762(4) . ? Ge1 O17 1.769(5) . ? Ge1 O25 1.784(4) 2_655 ? Ge2 O23 1.729(4) . ? Ge2 O6 1.743(4) . ? Ge2 O9 1.750(4) . ? Ge2 O22 1.762(3) . ? Ge3 O24 1.729(4) . ? Ge3 O14 1.737(4) . ? Ge3 O2 1.747(4) . ? Ge3 O25 1.761(4) . ? Ni1 N1 2.077(7) . ? Ni1 N4 2.082(8) . ? Ni1 N22' 2.10(2) . ? Ni1 N2 2.105(6) . ? Ni1 O5 2.121(5) 3_545 ? Ni1 N3 2.135(7) . ? Ni1 N22 2.192(10) . ? Ni2 N11 2.083(6) . ? Ni2 N12 2.088(6) . ? Ni2 N23 2.092(6) . ? Ni2 N14 2.100(6) . ? Ni2 N13 2.120(6) . ? Ni2 O13 2.157(4) . ? V1 O5 1.622(5) . ? V1 O4 1.890(4) . ? V1 O3 1.926(4) 2_655 ? V1 O1 1.994(4) . ? V1 O2 1.995(4) 2_655 ? V1 V2 2.8697(14) . ? V1 V4 3.0292(14) 2_655 ? V1 V7 3.0384(14) . ? V2 O8 1.604(4) . ? V2 O7 1.935(4) . ? V2 O4 1.942(4) . ? V2 O3 1.950(4) 2_655 ? V2 O6 2.030(4) 2_655 ? V2 V3 3.0949(15) . ? V3 O11 1.605(4) . ? V3 O7 1.911(4) . ? V3 O10 1.933(4) . ? V3 O9 2.005(4) . ? V3 O6 2.030(4) 2_655 ? V3 V5 2.8382(13) . ? V3 V4 3.0199(14) . ? V4 O12 1.606(5) . ? V4 O10 1.925(4) . ? V4 O3 1.932(4) . ? V4 O9 1.998(4) . ? V4 O2 2.015(4) . ? V4 V1 3.0292(14) 2_655 ? V5 O13 1.617(4) . ? V5 O7 1.910(4) . ? V5 O15 1.938(4) . ? V5 O10 1.946(4) . ? V5 O14 2.026(4) . ? V5 V6 3.0703(13) . ? V6 O18 1.615(4) . ? V6 O15 1.910(4) . ? V6 O16 1.944(4) 2_655 ? V6 O17 1.998(4) 2_655 ? V6 O14 2.002(4) . ? V6 V7 2.8942(15) . ? V6 V8 3.0285(11) . ? V7 O19 1.609(4) . ? V7 O4 1.933(4) . ? V7 O15 1.947(4) . ? V7 O16 1.959(4) 2_655 ? V7 O1 2.025(4) . ? V8 O20 1.615(6) . ? V8 O16 1.928(4) . ? V8 O16 1.928(4) 2_655 ? V8 O17 1.988(4) 2_655 ? V8 O17 1.988(4) . ? V8 V6 3.0285(11) 2_655 ? O2 V1 1.995(4) 2_655 ? O3 V1 1.926(4) 2_655 ? O3 V2 1.950(4) 2_655 ? O5 Ni1 2.121(5) 3_455 ? O6 V2 2.030(4) 2_655 ? O6 V3 2.030(4) 2_655 ? O16 V6 1.944(4) 2_655 ? O16 V7 1.959(4) 2_655 ? O17 V6 1.998(4) 2_655 ? O22 Ge2 1.762(3) 2_655 ? O25 Ge1 1.784(4) 2_655 ? N1 C1 1.481(10) . ? N1 C5 1.483(11) . ? N1 C3 1.487(10) . ? N2 C2 1.484(10) . ? N3 C4 1.481(11) . ? N4 C6 1.465(15) . ? C1 C2 1.524(11) . ? C3 C4 1.496(14) . ? C5 C6 1.520(17) . ? N11 C13 1.451(10) . ? N11 C15 1.492(9) . ? N11 C11 1.511(9) . ? N12 C12 1.501(10) . ? N13 C14 1.460(11) . ? N14 C16 1.489(10) . ? C11 C12 1.488(13) . ? C13 C14 1.536(13) . ? C15 C16 1.509(10) . ? N21 C21 1.478(9) . ? N21 C23 1.479(10) . ? N21 C25 1.493(10) . ? N22 C22 1.409(13) . ? N22' C22 1.39(2) . ? N23 C24 1.480(10) . ? N24 C26 1.482(12) . ? C21 C22 1.469(13) . ? C23 C24 1.510(10) . ? C25 C26 1.497(12) . ? 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 O21 Ge1 O1 117.1(2) . . ? O21 Ge1 O17 114.7(2) . . ? O1 Ge1 O17 105.7(2) . . ? O21 Ge1 O25 109.1(2) . 2_655 ? O1 Ge1 O25 105.25(19) . 2_655 ? O17 Ge1 O25 103.68(19) . 2_655 ? O23 Ge2 O6 110.1(2) . . ? O23 Ge2 O9 111.8(2) . . ? O6 Ge2 O9 109.95(19) . . ? O23 Ge2 O22 111.2(2) . . ? O6 Ge2 O22 107.59(17) . . ? O9 Ge2 O22 106.07(16) . . ? O24 Ge3 O14 113.1(2) . . ? O24 Ge3 O2 109.2(2) . . ? O14 Ge3 O2 110.7(2) . . ? O24 Ge3 O25 109.3(2) . . ? O14 Ge3 O25 107.4(2) . . ? O2 Ge3 O25 107.10(19) . . ? N1 Ni1 N4 83.5(3) . . ? N1 Ni1 N22' 166.5(7) . . ? N4 Ni1 N22' 87.1(7) . . ? N1 Ni1 N2 84.1(2) . . ? N4 Ni1 N2 91.0(3) . . ? N22' Ni1 N2 86.4(7) . . ? N1 Ni1 O5 90.7(2) . 3_545 ? N4 Ni1 O5 174.2(3) . 3_545 ? N22' Ni1 O5 98.6(7) . 3_545 ? N2 Ni1 O5 88.1(2) . 3_545 ? N1 Ni1 N3 82.0(3) . . ? N4 Ni1 N3 95.6(3) . . ? N22' Ni1 N3 108.6(7) . . ? N2 Ni1 N3 163.8(3) . . ? O5 Ni1 N3 83.8(3) 3_545 . ? N1 Ni1 N22 169.6(4) . . ? N4 Ni1 N22 106.9(4) . . ? N22' Ni1 N22 22.1(6) . . ? N2 Ni1 N22 95.5(3) . . ? O5 Ni1 N22 78.9(3) 3_545 . ? N3 Ni1 N22 96.7(4) . . ? N11 Ni2 N12 84.0(3) . . ? N11 Ni2 N23 176.7(2) . . ? N12 Ni2 N23 98.0(3) . . ? N11 Ni2 N14 84.0(2) . . ? N12 Ni2 N14 95.6(3) . . ? N23 Ni2 N14 98.4(2) . . ? N11 Ni2 N13 82.4(3) . . ? N12 Ni2 N13 163.0(3) . . ? N23 Ni2 N13 95.1(3) . . ? N14 Ni2 N13 93.1(3) . . ? N11 Ni2 O13 92.13(19) . . ? N12 Ni2 O13 84.1(2) . . ? N23 Ni2 O13 85.5(2) . . ? N14 Ni2 O13 176.1(2) . . ? N13 Ni2 O13 86.2(2) . . ? O5 V1 O4 111.0(2) . . ? O5 V1 O3 109.1(2) . 2_655 ? O4 V1 O3 83.58(18) . 2_655 ? O5 V1 O1 109.9(2) . . ? O4 V1 O1 79.13(17) . . ? O3 V1 O1 140.81(19) 2_655 . ? O5 V1 O2 106.0(2) . 2_655 ? O4 V1 O2 142.59(19) . 2_655 ? O3 V1 O2 79.47(17) 2_655 2_655 ? O1 V1 O2 93.47(17) . 2_655 ? O5 V1 V2 109.50(17) . . ? O4 V1 V2 42.21(13) . . ? O3 V1 V2 42.57(13) 2_655 . ? O1 V1 V2 117.72(13) . . ? O2 V1 V2 118.88(13) 2_655 . ? O5 V1 V4 111.64(17) . 2_655 ? O4 V1 V4 116.09(14) . 2_655 ? O3 V1 V4 38.33(13) 2_655 2_655 ? O1 V1 V4 124.95(13) . 2_655 ? O2 V1 V4 41.18(12) 2_655 2_655 ? V2 V1 V4 79.52(4) . 2_655 ? O5 V1 V7 115.89(17) . . ? O4 V1 V7 37.87(13) . . ? O3 V1 V7 114.87(14) 2_655 . ? O1 V1 V7 41.28(12) . . ? O2 V1 V7 125.66(13) 2_655 . ? V2 V1 V7 78.38(4) . . ? V4 V1 V7 131.91(4) 2_655 . ? O8 V2 O7 111.6(2) . . ? O8 V2 O4 105.5(2) . . ? O7 V2 O4 90.02(18) . . ? O8 V2 O3 109.3(2) . 2_655 ? O7 V2 O3 139.07(18) . 2_655 ? O4 V2 O3 81.59(17) . 2_655 ? O8 V2 O6 107.5(2) . 2_655 ? O7 V2 O6 76.42(17) . 2_655 ? O4 V2 O6 146.94(18) . 2_655 ? O3 V2 O6 89.15(17) 2_655 2_655 ? O8 V2 V1 105.63(19) . . ? O7 V2 V1 125.08(13) . . ? O4 V2 V1 40.83(13) . . ? O3 V2 V1 41.93(12) 2_655 . ? O6 V2 V1 127.96(12) 2_655 . ? O8 V2 V3 113.64(19) . . ? O7 V2 V3 36.15(12) . . ? O4 V2 V3 121.51(14) . . ? O3 V2 V3 120.74(13) 2_655 . ? O6 V2 V3 40.33(12) 2_655 . ? V1 V2 V3 140.68(4) . . ? O11 V3 O7 111.7(2) . . ? O11 V3 O10 108.8(2) . . ? O7 V3 O10 83.84(18) . . ? O11 V3 O9 109.7(2) . . ? O7 V3 O9 138.35(18) . . ? O10 V3 O9 79.20(17) . . ? O11 V3 O6 111.1(2) . 2_655 ? O7 V3 O6 76.93(17) . 2_655 ? O10 V3 O6 139.72(17) . 2_655 ? O9 V3 O6 92.14(18) . 2_655 ? O11 V3 V5 109.51(18) . . ? O7 V3 V5 42.01(13) . . ? O10 V3 V5 43.14(12) . . ? O9 V3 V5 117.81(12) . . ? O6 V3 V5 115.53(12) 2_655 . ? O11 V3 V4 112.78(19) . . ? O7 V3 V4 115.29(13) . . ? O10 V3 V4 38.39(12) . . ? O9 V3 V4 40.95(12) . . ? O6 V3 V4 124.04(13) 2_655 . ? V5 V3 V4 79.74(4) . . ? O11 V3 V2 116.15(19) . . ? O7 V3 V2 36.67(13) . . ? O10 V3 V2 114.36(13) . . ? O9 V3 V2 122.50(13) . . ? O6 V3 V2 40.32(12) 2_655 . ? V5 V3 V2 77.20(4) . . ? V4 V3 V2 130.42(4) . . ? O12 V4 O10 115.3(2) . . ? O12 V4 O3 112.1(2) . . ? O10 V4 O3 132.57(18) . . ? O12 V4 O9 106.4(2) . . ? O10 V4 O9 79.54(17) . . ? O3 V4 O9 89.28(18) . . ? O12 V4 O2 102.4(2) . . ? O10 V4 O2 89.28(17) . . ? O3 V4 O2 78.85(17) . . ? O9 V4 O2 151.21(18) . . ? O12 V4 V3 115.12(18) . . ? O10 V4 V3 38.57(12) . . ? O3 V4 V3 118.41(14) . . ? O9 V4 V3 41.11(12) . . ? O2 V4 V3 124.48(13) . . ? O12 V4 V1 111.17(18) . 2_655 ? O10 V4 V1 117.35(13) . 2_655 ? O3 V4 V1 38.20(12) . 2_655 ? O9 V4 V1 123.70(13) . 2_655 ? O2 V4 V1 40.69(12) . 2_655 ? V3 V4 V1 133.71(4) . 2_655 ? O13 V5 O7 106.2(2) . . ? O13 V5 O15 106.5(2) . . ? O7 V5 O15 90.76(18) . . ? O13 V5 O10 110.7(2) . . ? O7 V5 O10 83.53(18) . . ? O15 V5 O10 142.50(17) . . ? O13 V5 O14 105.6(2) . . ? O7 V5 O14 147.92(18) . . ? O15 V5 O14 76.78(17) . . ? O10 V5 O14 88.68(17) . . ? O13 V5 V3 106.87(15) . . ? O7 V5 V3 42.04(13) . . ? O15 V5 V3 128.13(13) . . ? O10 V5 V3 42.79(12) . . ? O14 V5 V3 128.69(12) . . ? O13 V5 V6 109.67(15) . . ? O7 V5 V6 122.59(13) . . ? O15 V5 V6 36.77(12) . . ? O10 V5 V6 121.35(13) . . ? O14 V5 V6 40.04(12) . . ? V3 V5 V6 143.43(4) . . ? O18 V6 O15 109.9(2) . . ? O18 V6 O16 111.9(2) . 2_655 ? O15 V6 O16 83.22(18) . 2_655 ? O18 V6 O17 111.7(2) . 2_655 ? O15 V6 O17 138.28(18) . 2_655 ? O16 V6 O17 78.76(18) 2_655 2_655 ? O18 V6 O14 107.3(2) . . ? O15 V6 O14 77.98(18) . . ? O16 V6 O14 140.32(18) 2_655 . ? O17 V6 O14 92.57(18) 2_655 . ? O18 V6 V7 111.4(2) . . ? O15 V6 V7 41.87(13) . . ? O16 V6 V7 42.35(13) 2_655 . ? O17 V6 V7 116.35(13) 2_655 . ? O14 V6 V7 116.08(13) . . ? O18 V6 V8 117.60(18) . . ? O15 V6 V8 113.93(13) . . ? O16 V6 V8 38.35(13) 2_655 . ? O17 V6 V8 40.44(12) 2_655 . ? O14 V6 V8 123.31(13) . . ? V7 V6 V8 78.35(3) . . ? O18 V6 V5 113.22(18) . . ? O15 V6 V5 37.39(13) . . ? O16 V6 V5 114.18(13) 2_655 . ? O17 V6 V5 122.45(13) 2_655 . ? O14 V6 V5 40.61(12) . . ? V7 V6 V5 77.44(4) . . ? V8 V6 V5 128.69(4) . . ? O19 V7 O4 109.0(2) . . ? O19 V7 O15 107.0(2) . . ? O4 V7 O15 89.92(18) . . ? O19 V7 O16 108.6(2) . 2_655 ? O4 V7 O16 142.20(19) . 2_655 ? O15 V7 O16 81.86(17) . 2_655 ? O19 V7 O1 106.3(2) . . ? O4 V7 O1 77.36(17) . . ? O15 V7 O1 146.63(18) . . ? O16 V7 O1 89.52(18) 2_655 . ? O19 V7 V6 106.92(18) . . ? O4 V7 V6 125.87(14) . . ? O15 V7 V6 40.91(12) . . ? O16 V7 V6 41.93(12) 2_655 . ? O1 V7 V6 127.88(13) . . ? O19 V7 V1 111.82(18) . . ? O4 V7 V1 36.89(13) . . ? O15 V7 V1 121.49(13) . . ? O16 V7 V1 122.12(13) 2_655 . ? O1 V7 V1 40.50(12) . . ? V6 V7 V1 141.22(4) . . ? O20 V8 O16 110.86(13) . . ? O20 V8 O16 110.86(13) . 2_655 ? O16 V8 O16 138.3(3) . 2_655 ? O20 V8 O17 104.20(13) . 2_655 ? O16 V8 O17 90.57(18) . 2_655 ? O16 V8 O17 79.36(18) 2_655 2_655 ? O20 V8 O17 104.20(13) . . ? O16 V8 O17 79.36(18) . . ? O16 V8 O17 90.57(18) 2_655 . ? O17 V8 O17 151.6(3) 2_655 . ? O20 V8 V6 111.98(3) . . ? O16 V8 V6 120.91(13) . . ? O16 V8 V6 38.72(13) 2_655 . ? O17 V8 V6 40.67(13) 2_655 . ? O17 V8 V6 125.09(13) . . ? O20 V8 V6 111.98(3) . 2_655 ? O16 V8 V6 38.72(13) . 2_655 ? O16 V8 V6 120.91(13) 2_655 2_655 ? O17 V8 V6 125.09(13) 2_655 2_655 ? O17 V8 V6 40.67(13) . 2_655 ? V6 V8 V6 136.04(6) . 2_655 ? Ge1 O1 V1 135.1(2) . . ? Ge1 O1 V7 125.6(2) . . ? V1 O1 V7 98.22(18) . . ? Ge3 O2 V1 132.2(2) . 2_655 ? Ge3 O2 V4 125.4(2) . . ? V1 O2 V4 98.13(17) 2_655 . ? V1 O3 V4 103.5(2) 2_655 . ? V1 O3 V2 95.50(18) 2_655 2_655 ? V4 O3 V2 152.9(3) . 2_655 ? V1 O4 V7 105.2(2) . . ? V1 O4 V2 96.96(19) . . ? V7 O4 V2 149.1(3) . . ? V1 O5 Ni1 151.0(3) . 3_455 ? Ge2 O6 V2 125.9(2) . 2_655 ? Ge2 O6 V3 132.7(2) . 2_655 ? V2 O6 V3 99.35(17) 2_655 2_655 ? V5 O7 V3 95.95(19) . . ? V5 O7 V2 149.3(2) . . ? V3 O7 V2 107.2(2) . . ? Ge2 O9 V4 125.7(2) . . ? Ge2 O9 V3 134.0(2) . . ? V4 O9 V3 97.95(18) . . ? V4 O10 V3 103.04(19) . . ? V4 O10 V5 152.3(2) . . ? V3 O10 V5 94.07(19) . . ? V5 O13 Ni2 148.7(3) . . ? Ge3 O14 V6 132.2(2) . . ? Ge3 O14 V5 126.6(2) . . ? V6 O14 V5 99.35(19) . . ? V6 O15 V5 105.8(2) . . ? V6 O15 V7 97.22(18) . . ? V5 O15 V7 147.9(2) . . ? V8 O16 V6 102.9(2) . 2_655 ? V8 O16 V7 148.7(2) . 2_655 ? V6 O16 V7 95.72(18) 2_655 2_655 ? Ge1 O17 V8 124.9(2) . . ? Ge1 O17 V6 134.7(2) . 2_655 ? V8 O17 V6 98.9(2) . 2_655 ? Ge2 O22 Ge2 115.2(3) . 2_655 ? Ge3 O25 Ge1 117.1(2) . 2_655 ? C1 N1 C5 111.9(7) . . ? C1 N1 C3 111.5(7) . . ? C5 N1 C3 112.5(7) . . ? C1 N1 Ni1 105.3(4) . . ? C5 N1 Ni1 109.7(6) . . ? C3 N1 Ni1 105.5(5) . . ? C2 N2 Ni1 109.0(5) . . ? C4 N3 Ni1 109.9(5) . . ? C6 N4 Ni1 106.8(6) . . ? N1 C1 C2 110.3(7) . . ? N2 C2 C1 109.4(6) . . ? N1 C3 C4 110.3(8) . . ? N3 C4 C3 110.8(8) . . ? N1 C5 C6 112.6(8) . . ? N4 C6 C5 109.7(8) . . ? C13 N11 C15 112.9(6) . . ? C13 N11 C11 110.8(6) . . ? C15 N11 C11 111.6(6) . . ? C13 N11 Ni2 106.8(5) . . ? C15 N11 Ni2 109.1(4) . . ? C11 N11 Ni2 105.3(5) . . ? C12 N12 Ni2 109.2(5) . . ? C14 N13 Ni2 110.1(5) . . ? C16 N14 Ni2 105.9(4) . . ? C12 C11 N11 109.7(6) . . ? C11 C12 N12 109.9(6) . . ? N11 C13 C14 110.6(7) . . ? N13 C14 C13 112.0(7) . . ? N11 C15 C16 112.1(6) . . ? N14 C16 C15 109.5(6) . . ? C21 N21 C23 110.5(6) . . ? C21 N21 C25 113.2(7) . . ? C23 N21 C25 116.3(6) . . ? C22 N22 Ni1 123.7(8) . . ? C22 N22' Ni1 131.8(15) . . ? C24 N23 Ni2 113.2(5) . . ? C22 C21 N21 114.7(8) . . ? N22' C22 N22 34.4(9) . . ? N22' C22 C21 115.4(12) . . ? N22 C22 C21 114.7(9) . . ? N21 C23 C24 112.9(6) . . ? N23 C24 C23 112.6(7) . . ? N21 C25 C26 117.6(7) . . ? N24 C26 C25 109.9(8) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.513 _refine_diff_density_min -1.059 _refine_diff_density_rms 0.142 _database_code_depnum_ccdc_archive 'CCDC 936481'