#------------------------------------------------------------------------------ #$Date: 2014-08-22 02:39:47 +0300 (Fri, 22 Aug 2014) $ #$Revision: 122327 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/21/77/7217797.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_7217797 loop_ _publ_author_name 'Ren, Xiaoyan' 'Pan, Qin He' 'Liu, Jianchong' 'Li, Yi' 'Wang, Fuxiang' 'Li, Jiyang' 'Xu, Yan' 'Li, Li' _publ_section_title ; A Family of Germanates Constructed from Ge7 Clusters Co-templated by Metal Complexes and Organic/Inorganic Species ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/C4CE00671B _journal_year 2014 _chemical_formula_moiety '[Ni (C4H14N3)2]2 Cl [Ge7O13(OH)2F3)]' _chemical_formula_sum 'C16 H54 Cl F3 Ge7 N12 Ni2 O15' _chemical_formula_weight 1372.71 _space_group_IT_number 13 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yac' _symmetry_space_group_name_H-M 'P 1 2/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _audit_update_record ; 2014-07-20 # Formatted by publCIF ; _cell_angle_alpha 90.00 _cell_angle_beta 101.292(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 8.8785(7) _cell_length_b 17.4501(14) _cell_length_c 13.1922(11) _cell_measurement_temperature 293(2) _cell_volume 2004.3(3) _computing_cell_refinement Process-auto _computing_data_collection Process-auto _computing_data_reduction Process-auto _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXP-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0782 _diffrn_reflns_av_sigmaI/netI 0.1069 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 11746 _diffrn_reflns_theta_full 26.35 _diffrn_reflns_theta_max 26.35 _diffrn_reflns_theta_min 1.17 _exptl_absorpt_coefficient_mu 6.244 _exptl_absorpt_correction_T_max 0.7883 _exptl_absorpt_correction_T_min 0.5579 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour red _exptl_crystal_density_diffrn 2.275 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1356 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.948 _refine_diff_density_min -0.775 _refine_diff_density_rms 0.146 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 258 _refine_ls_number_reflns 4088 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.032 _refine_ls_R_factor_all 0.0806 _refine_ls_R_factor_gt 0.0410 _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/[\s^2^(Fo^2^)+(0.0091P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0687 _refine_ls_wR_factor_ref 0.0894 _reflns_number_gt 2416 _reflns_number_total 4088 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL a in P2/n CELL 0.71073 8.8785 17.4501 13.1922 90.000 101.292 90.000 ZERR 2.00 0.0007 0.0014 0.0011 0.000 0.002 0.000 LATT 1 SYMM 0.5-X, Y, 0.5-Z SFAC C H N O F NI GE cl UNIT 32 108 24 30 6 4 14 2 TEMP 0 L.S. 4 BOND $h eqiv $1 -x+1, -y, -z+1 eqiv $2 x+1/2, -y, z+1/2 eqiv $3 -x+1, -y+1, -z+1 eqiv $4 -x+1/2, y, -z+3/2 htab N1 O6_$1 htab N2 F2 htab N3 F2_$2 htab N4 F1_$3 htab N5 O3_$4 htab N6 O2_$3 FMAP 2 omit -2 52.7 PLAN -20 acta WGHT 0.009050 FVAR 0.12012 GE1 7 0.250000 0.336048 0.750000 10.50000 0.01690 0.02154 = 0.02431 0.00000 0.00582 0.00000 GE2 7 0.319909 0.142274 0.661656 11.00000 0.01969 0.02407 = 0.02220 -0.00103 0.00473 0.00138 GE3 7 0.079127 0.256554 0.549092 11.00000 0.02099 0.03051 = 0.02302 0.00048 0.00406 0.00287 GE4 7 -0.066515 0.256026 0.738233 11.00000 0.01481 0.02573 = 0.02819 -0.00067 0.00655 -0.00009 NI1 6 0.750000 -0.061129 0.750000 10.50000 0.03367 0.03513 = 0.02738 0.00000 0.01366 0.00000 NI2 6 0.500000 0.500000 0.500000 10.50000 0.02647 0.02859 = 0.03008 0.00632 0.00635 -0.00148 CL1 8 0.750000 -0.328360 0.750000 10.50000 0.06588 0.04414 = 0.04431 0.00000 -0.00068 0.00000 F1 5 0.250000 0.439579 0.750000 10.50000 0.02460 0.02725 = 0.04761 0.00000 0.01360 0.00000 F2 5 0.372173 0.060196 0.591191 11.00000 0.03462 0.03431 = 0.03558 -0.00595 0.00830 0.00580 O1 4 0.250000 0.221482 0.750000 10.50000 0.01332 0.02616 = 0.01357 0.00000 0.00069 0.00000 O2 4 0.173776 0.335904 0.607024 11.00000 0.02262 0.02364 = 0.02430 0.00408 0.00512 -0.00061 O3 4 0.048684 0.334445 0.777002 11.00000 0.01740 0.02543 = 0.03270 -0.00305 0.00812 -0.00403 O4 4 0.513379 0.173779 0.687259 11.00000 0.02200 0.03185 = 0.02748 -0.00299 0.00820 -0.00118 O5 4 0.250000 0.080573 0.750000 10.50000 0.01709 0.01937 = 0.02794 0.00000 0.00421 0.00000 O6 4 0.196630 0.176491 0.548105 11.00000 0.03093 0.03572 = 0.02038 -0.00343 0.00492 0.01002 O7 4 -0.000047 0.277011 0.419572 11.00000 0.03646 0.05779 = 0.02039 0.00711 -0.00079 0.00478 AFIX 81 H7 2 0.069021 0.287211 0.388627 11.00000 10.08000 AFIX 0 O8 4 -0.075983 0.233187 0.607685 11.00000 0.02359 0.03187 = 0.03386 -0.00183 0.01207 -0.00562 O9 4 -0.250000 0.284633 0.750000 10.50000 0.01216 0.03956 = 0.04439 0.00000 0.01201 0.00000 N1 3 0.670220 -0.151031 0.639319 11.00000 0.04343 0.04642 = 0.03495 0.00492 0.02091 -0.00060 AFIX 21 H1A 2 0.706338 -0.143460 0.580946 11.00000 -1.20000 H1B 2 0.703228 -0.196988 0.665674 11.00000 -1.20000 AFIX 0 N2 3 0.519249 -0.056799 0.756022 11.00000 0.03604 0.05445 = 0.03119 0.01612 0.01602 0.01739 AFIX 11 H2 2 0.475685 -0.018402 0.713511 11.00000 -1.20000 AFIX 0 N3 3 0.767781 0.019283 0.873097 11.00000 0.05490 0.04676 = 0.03534 -0.00599 0.01448 0.00391 AFIX 21 H3A 2 0.825624 -0.000138 0.931087 11.00000 -1.20000 H3B 2 0.812069 0.062792 0.856847 11.00000 -1.20000 AFIX 0 N4 3 0.551687 0.460828 0.356302 11.00000 0.03924 0.04997 = 0.04334 0.00114 0.00971 -0.00719 AFIX 21 H4A 2 0.464026 0.448174 0.312705 11.00000 -1.20000 H4B 2 0.597083 0.498770 0.327102 11.00000 -1.20000 AFIX 0 N5 3 0.645924 0.411630 0.558729 11.00000 0.04369 0.03769 = 0.04804 0.00328 0.00162 -0.00031 AFIX 11 H5 2 0.609037 0.388573 0.610748 11.00000 -1.20000 AFIX 0 N6 3 0.700098 0.564718 0.530055 11.00000 0.04431 0.04364 = 0.03231 -0.00289 0.01574 -0.01308 AFIX 21 H6A 2 0.705163 0.594760 0.475369 11.00000 -1.20000 H6B 2 0.700085 0.595071 0.585210 11.00000 -1.20000 AFIX 0 C1 1 0.500594 -0.148404 0.617155 11.00000 0.04571 0.06094 = 0.05452 -0.01440 0.01230 -0.01229 AFIX 21 H1C 2 0.459521 -0.197396 0.590016 11.00000 -1.20000 H1D 2 0.464936 -0.109311 0.565782 11.00000 -1.20000 AFIX 0 C2 1 0.446743 -0.130682 0.714452 11.00000 0.03235 0.05113 = 0.07678 -0.00627 0.02019 -0.00900 AFIX 21 H2A 2 0.476151 -0.171464 0.764367 11.00000 -1.20000 H2B 2 0.335739 -0.126004 0.700811 11.00000 -1.20000 AFIX 0 C3 1 0.511764 -0.035325 0.862369 11.00000 0.05596 0.06106 = 0.04068 0.01534 0.02796 0.02655 AFIX 21 H3C 2 0.549629 -0.076860 0.909351 11.00000 -1.20000 H3D 2 0.406489 -0.024464 0.867798 11.00000 -1.20000 AFIX 0 C4 1 0.610365 0.035198 0.889365 11.00000 0.07167 0.05274 = 0.03294 0.00132 0.02316 0.03246 AFIX 21 H4C 2 0.566673 0.077776 0.846152 11.00000 -1.20000 H4D 2 0.613657 0.049098 0.960958 11.00000 -1.20000 AFIX 0 C5 1 0.653517 0.394291 0.373301 11.00000 0.04221 0.07155 = 0.06603 -0.02592 0.02162 0.00017 AFIX 21 H5A 2 0.758677 0.410156 0.374952 11.00000 -1.20000 H5B 2 0.624619 0.357853 0.317343 11.00000 -1.20000 AFIX 0 C6 1 0.640792 0.357190 0.475228 11.00000 0.03471 0.03939 = 0.08602 -0.00063 0.00059 0.01575 AFIX 21 H6C 2 0.545032 0.328908 0.466169 11.00000 -1.20000 H6D 2 0.724111 0.320795 0.494266 11.00000 -1.20000 AFIX 0 C7 1 0.798282 0.442305 0.600533 11.00000 0.04490 0.05062 = 0.07689 0.00279 -0.01747 0.00988 AFIX 21 H7A 2 0.874545 0.404050 0.592908 11.00000 -1.20000 H7B 2 0.806465 0.451832 0.673850 11.00000 -1.20000 AFIX 0 C8 1 0.833071 0.513393 0.550492 11.00000 0.02820 0.06276 = 0.08284 -0.00779 0.01013 0.00033 AFIX 21 H8A 2 0.918109 0.539247 0.594669 11.00000 -1.20000 H8B 2 0.864167 0.501156 0.485864 11.00000 -1.20000 HKLF 4 REM a in P2/n REM R1 = 0.0423 for 2536 Fo > 4sig(Fo) and 0.0909 for all 4577 data REM 258 parameters refined using 0 restraints END ; _[local]_cod_data_source_file c4ce00671b2.cif _[local]_cod_data_source_block a _[local]_cod_cif_authors_sg_H-M P2/n _cod_database_code 7217797 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, 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 Ge1 Ge 0.2500 0.33605(6) 0.7500 0.0207(3) Uani 1 2 d S Ge2 Ge 0.31991(9) 0.14227(4) 0.66166(6) 0.0219(2) Uani 1 1 d . Ge3 Ge 0.07913(8) 0.25656(5) 0.54910(6) 0.0249(2) Uani 1 1 d . Ge4 Ge -0.06651(8) 0.25603(4) 0.73824(6) 0.0226(2) Uani 1 1 d . Ni1 Ni 0.7500 -0.06113(8) 0.7500 0.0311(4) Uani 1 2 d S Ni2 Ni 0.5000 0.5000 0.5000 0.0284(4) Uani 1 2 d S Cl1 Cl 0.7500 -0.32835(18) 0.7500 0.0530(9) Uani 1 2 d S F1 F 0.2500 0.4396(3) 0.7500 0.0323(16) Uani 1 2 d S F2 F 0.3722(4) 0.0602(2) 0.5912(3) 0.0348(11) Uani 1 1 d . O1 O 0.2500 0.2215(3) 0.7500 0.0180(16) Uani 1 2 d S O2 O 0.1738(5) 0.3359(3) 0.6070(3) 0.0233(12) Uani 1 1 d . O3 O 0.0487(5) 0.3345(3) 0.7770(3) 0.0248(12) Uani 1 1 d . O4 O 0.5134(5) 0.1738(3) 0.6872(4) 0.0268(12) Uani 1 1 d . O5 O 0.2500 0.0806(3) 0.7500 0.0214(17) Uani 1 2 d S O6 O 0.1967(5) 0.1765(3) 0.5481(3) 0.0290(13) Uani 1 1 d . O7 O -0.0001(5) 0.2770(3) 0.4196(4) 0.0391(15) Uani 1 1 d . H7 H 0.0690 0.2872 0.3886 0.080 Uiso 1 1 calc . O8 O -0.0760(5) 0.2332(3) 0.6077(4) 0.0289(13) Uani 1 1 d . O9 O -0.2500 0.2846(4) 0.7500 0.0310(19) Uani 1 2 d S N1 N 0.6702(7) -0.1510(4) 0.6393(5) 0.0395(18) Uani 1 1 d . H1A H 0.7064 -0.1435 0.5809 0.047 Uiso 1 1 calc . H1B H 0.7032 -0.1970 0.6657 0.047 Uiso 1 1 calc . N2 N 0.5192(7) -0.0568(4) 0.7560(5) 0.0394(19) Uani 1 1 d . H2 H 0.4756 -0.0184 0.7135 0.047 Uiso 1 1 calc . N3 N 0.7678(8) 0.0193(4) 0.8731(5) 0.0446(19) Uani 1 1 d . H3A H 0.8256 -0.0001 0.9311 0.053 Uiso 1 1 calc . H3B H 0.8121 0.0628 0.8569 0.053 Uiso 1 1 calc . N4 N 0.5517(7) 0.4609(4) 0.3563(5) 0.0441(19) Uani 1 1 d . H4A H 0.4640 0.4482 0.3127 0.053 Uiso 1 1 calc . H4B H 0.5971 0.4988 0.3271 0.053 Uiso 1 1 calc . N5 N 0.6460(8) 0.4116(4) 0.5587(6) 0.0441(19) Uani 1 1 d . H5 H 0.6091 0.3886 0.6107 0.053 Uiso 1 1 calc . N6 N 0.7001(7) 0.5647(4) 0.5301(5) 0.0388(18) Uani 1 1 d . H6A H 0.7051 0.5948 0.4754 0.047 Uiso 1 1 calc . H6B H 0.7001 0.5951 0.5852 0.047 Uiso 1 1 calc . C1 C 0.5006(10) -0.1484(5) 0.6171(7) 0.054(3) Uani 1 1 d . H1C H 0.4595 -0.1974 0.5900 0.064 Uiso 1 1 calc . H1D H 0.4649 -0.1093 0.5658 0.064 Uiso 1 1 calc . C2 C 0.4468(9) -0.1307(5) 0.7144(8) 0.052(3) Uani 1 1 d . H2A H 0.4763 -0.1715 0.7643 0.062 Uiso 1 1 calc . H2B H 0.3358 -0.1261 0.7008 0.062 Uiso 1 1 calc . C3 C 0.5117(10) -0.0354(6) 0.8624(7) 0.050(3) Uani 1 1 d . H3C H 0.5496 -0.0769 0.9094 0.060 Uiso 1 1 calc . H3D H 0.4064 -0.0245 0.8678 0.060 Uiso 1 1 calc . C4 C 0.6103(11) 0.0352(5) 0.8893(7) 0.051(3) Uani 1 1 d . H4C H 0.5666 0.0777 0.8460 0.061 Uiso 1 1 calc . H4D H 0.6135 0.0491 0.9609 0.061 Uiso 1 1 calc . C5 C 0.6535(10) 0.3943(6) 0.3733(8) 0.059(3) Uani 1 1 d . H5A H 0.7586 0.4102 0.3749 0.070 Uiso 1 1 calc . H5B H 0.6245 0.3579 0.3173 0.070 Uiso 1 1 calc . C6 C 0.6408(9) 0.3572(5) 0.4752(8) 0.055(3) Uani 1 1 d . H6C H 0.5451 0.3289 0.4662 0.066 Uiso 1 1 calc . H6D H 0.7242 0.3208 0.4942 0.066 Uiso 1 1 calc . C7 C 0.7983(10) 0.4423(6) 0.6005(8) 0.062(3) Uani 1 1 d . H7A H 0.8745 0.4040 0.5929 0.074 Uiso 1 1 calc . H7B H 0.8064 0.4518 0.6738 0.074 Uiso 1 1 calc . C8 C 0.8332(10) 0.5134(6) 0.5505(8) 0.058(3) Uani 1 1 d . H8A H 0.9182 0.5393 0.5946 0.070 Uiso 1 1 calc . H8B H 0.8642 0.5012 0.4858 0.070 Uiso 1 1 calc . 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 0.0170(6) 0.0216(6) 0.0244(7) 0.000 0.0059(5) 0.000 Ge2 0.0197(4) 0.0242(4) 0.0222(5) -0.0011(4) 0.0048(3) 0.0014(4) Ge3 0.0210(5) 0.0306(5) 0.0232(5) 0.0005(4) 0.0041(4) 0.0029(4) Ge4 0.0149(4) 0.0258(5) 0.0282(5) -0.0007(4) 0.0066(3) -0.0001(4) Ni1 0.0338(9) 0.0352(9) 0.0274(9) 0.000 0.0136(7) 0.000 Ni2 0.0267(8) 0.0286(8) 0.0301(9) 0.0063(7) 0.0063(7) -0.0015(7) Cl1 0.066(2) 0.044(2) 0.044(2) 0.000 -0.0007(17) 0.000 F1 0.025(3) 0.027(3) 0.047(4) 0.000 0.014(3) 0.000 F2 0.035(3) 0.035(3) 0.036(3) -0.006(2) 0.008(2) 0.006(2) O1 0.013(4) 0.026(4) 0.013(4) 0.000 0.001(3) 0.000 O2 0.022(3) 0.024(3) 0.024(3) 0.004(2) 0.005(2) -0.001(2) O3 0.017(3) 0.026(3) 0.033(3) -0.003(2) 0.008(2) -0.004(2) O4 0.022(3) 0.032(3) 0.027(3) -0.003(3) 0.008(2) -0.001(2) O5 0.017(4) 0.019(4) 0.029(4) 0.000 0.004(3) 0.000 O6 0.031(3) 0.036(3) 0.020(3) -0.004(3) 0.005(2) 0.010(2) O7 0.036(3) 0.058(4) 0.021(3) 0.007(3) -0.001(2) 0.005(3) O8 0.023(3) 0.032(3) 0.034(3) -0.002(3) 0.012(2) -0.005(2) O9 0.012(4) 0.040(5) 0.044(5) 0.000 0.012(3) 0.000 N1 0.043(4) 0.047(4) 0.035(4) 0.005(4) 0.021(3) -0.001(4) N2 0.036(4) 0.056(5) 0.031(4) 0.016(4) 0.016(3) 0.018(4) N3 0.055(5) 0.047(5) 0.035(5) -0.006(4) 0.015(4) 0.004(4) N4 0.039(4) 0.050(5) 0.043(5) 0.001(4) 0.009(4) -0.007(4) N5 0.044(5) 0.038(4) 0.048(5) 0.003(4) 0.002(4) 0.000(4) N6 0.044(4) 0.044(4) 0.032(4) -0.003(4) 0.016(3) -0.013(4) C1 0.046(6) 0.061(7) 0.055(7) -0.014(6) 0.012(5) -0.012(5) C2 0.032(5) 0.051(6) 0.077(8) -0.007(6) 0.020(5) -0.010(5) C3 0.056(6) 0.061(7) 0.042(6) 0.015(5) 0.028(5) 0.026(5) C4 0.072(7) 0.053(6) 0.032(6) 0.001(5) 0.023(5) 0.033(6) C5 0.042(6) 0.072(7) 0.066(8) -0.026(6) 0.022(5) 0.000(5) C6 0.035(6) 0.040(6) 0.086(8) 0.000(6) 0.000(5) 0.016(5) C7 0.045(6) 0.051(6) 0.077(8) 0.003(6) -0.018(6) 0.010(5) C8 0.029(5) 0.063(7) 0.082(8) -0.007(6) 0.010(5) 0.000(5) 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' F F 0.0171 0.0103 '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' Cl Cl 0.1484 0.1585 '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 F1 Ge1 O2 90.08(14) . . F1 Ge1 O2 90.08(14) . 2_556 O2 Ge1 O2 179.8(3) . 2_556 F1 Ge1 O3 90.84(14) . . O2 Ge1 O3 91.21(19) . . O2 Ge1 O3 88.79(19) 2_556 . F1 Ge1 O3 90.84(14) . 2_556 O2 Ge1 O3 88.79(19) . 2_556 O2 Ge1 O3 91.21(19) 2_556 2_556 O3 Ge1 O3 178.3(3) . 2_556 F1 Ge1 O1 180 . . O2 Ge1 O1 89.92(14) . . O2 Ge1 O1 89.92(14) 2_556 . O3 Ge1 O1 89.16(14) . . O3 Ge1 O1 89.16(14) 2_556 . O4 Ge2 O6 118.1(2) . . O4 Ge2 O5 120.73(16) . . O6 Ge2 O5 121.18(16) . . O4 Ge2 F2 90.4(2) . . O6 Ge2 F2 90.61(19) . . O5 Ge2 F2 90.9(2) . . O4 Ge2 O1 94.30(17) . . O6 Ge2 O1 92.81(17) . . O5 Ge2 O1 81.3(2) . . F2 Ge2 O1 172.07(19) . . O4 Ge2 Ge2 113.95(16) . 2_556 O6 Ge2 Ge2 113.25(16) . 2_556 O5 Ge2 Ge2 37.09(16) . 2_556 F2 Ge2 Ge2 127.94(14) . 2_556 O1 Ge2 Ge2 44.16(13) . 2_556 O2 Ge3 O6 114.0(2) . . O2 Ge3 O7 109.7(2) . . O6 Ge3 O7 106.4(2) . . O2 Ge3 O8 110.4(2) . . O6 Ge3 O8 109.8(2) . . O7 Ge3 O8 106.1(2) . . O3 Ge4 O9 104.9(3) . . O3 Ge4 O4 113.9(2) . 2_556 O9 Ge4 O4 109.8(2) . 2_556 O3 Ge4 O8 112.5(2) . . O9 Ge4 O8 106.69(15) . . O4 Ge4 O8 108.7(2) 2_556 . N2 Ni1 N2 175.8(4) . 2_656 N2 Ni1 N3 94.5(3) . 2_656 N2 Ni1 N3 82.7(3) 2_656 2_656 N2 Ni1 N3 82.7(3) . . N2 Ni1 N3 94.5(3) 2_656 . N3 Ni1 N3 97.5(4) 2_656 . N2 Ni1 N1 81.8(3) . . N2 Ni1 N1 101.3(2) 2_656 . N3 Ni1 N1 89.9(2) 2_656 . N3 Ni1 N1 163.3(3) . . N2 Ni1 N1 101.3(2) . 2_656 N2 Ni1 N1 81.8(3) 2_656 2_656 N3 Ni1 N1 163.3(2) 2_656 2_656 N3 Ni1 N1 89.9(2) . 2_656 N1 Ni1 N1 87.2(3) . 2_656 N5 Ni2 N5 180 3_666 . N5 Ni2 N6 96.7(3) 3_666 . N5 Ni2 N6 83.3(3) . . N5 Ni2 N6 83.3(3) 3_666 3_666 N5 Ni2 N6 96.7(3) . 3_666 N6 Ni2 N6 180 . 3_666 N5 Ni2 N4 97.7(3) 3_666 . N5 Ni2 N4 82.3(3) . . N6 Ni2 N4 91.1(2) . . N6 Ni2 N4 88.9(2) 3_666 . N5 Ni2 N4 82.3(3) 3_666 3_666 N5 Ni2 N4 97.7(3) . 3_666 N6 Ni2 N4 88.9(2) . 3_666 N6 Ni2 N4 91.1(2) 3_666 3_666 N4 Ni2 N4 180 . 3_666 Ge2 O1 Ge2 91.7(3) . 2_556 Ge2 O1 Ge1 134.16(13) . . Ge2 O1 Ge1 134.16(13) 2_556 . Ge3 O2 Ge1 119.8(2) . . Ge4 O3 Ge1 118.9(3) . . Ge4 O4 Ge2 120.4(3) 2_556 . Ge2 O5 Ge2 105.8(3) 2_556 . Ge3 O6 Ge2 122.2(3) . . Ge3 O7 H7 109.5 . . Ge4 O8 Ge3 119.3(2) . . Ge4 O9 Ge4 146.7(4) . 2_456 C1 N1 Ni1 107.3(5) . . C1 N1 H1A 110.3 . . Ni1 N1 H1A 110.3 . . C1 N1 H1B 110.3 . . Ni1 N1 H1B 110.3 . . H1A N1 H1B 108.5 . . C3 N2 C2 118.3(7) . . C3 N2 Ni1 106.1(5) . . C2 N2 Ni1 108.2(5) . . C3 N2 H2 108.0 . . C2 N2 H2 108.0 . . Ni1 N2 H2 108.0 . . C4 N3 Ni1 107.6(5) . . C4 N3 H3A 110.2 . . Ni1 N3 H3A 110.2 . . C4 N3 H3B 110.2 . . Ni1 N3 H3B 110.2 . . H3A N3 H3B 108.5 . . C5 N4 Ni2 110.5(5) . . C5 N4 H4A 109.6 . . Ni2 N4 H4A 109.6 . . C5 N4 H4B 109.6 . . Ni2 N4 H4B 109.6 . . H4A N4 H4B 108.1 . . C6 N5 C7 114.6(7) . . C6 N5 Ni2 106.3(5) . . C7 N5 Ni2 109.6(5) . . C6 N5 H5 108.7 . . C7 N5 H5 108.7 . . Ni2 N5 H5 108.7 . . C8 N6 Ni2 109.4(5) . . C8 N6 H6A 109.8 . . Ni2 N6 H6A 109.8 . . C8 N6 H6B 109.8 . . Ni2 N6 H6B 109.8 . . H6A N6 H6B 108.2 . . N1 C1 C2 108.8(7) . . N1 C1 H1C 109.9 . . C2 C1 H1C 109.9 . . N1 C1 H1D 109.9 . . C2 C1 H1D 109.9 . . H1C C1 H1D 108.3 . . C1 C2 N2 107.9(7) . . C1 C2 H2A 110.1 . . N2 C2 H2A 110.1 . . C1 C2 H2B 110.1 . . N2 C2 H2B 110.1 . . H2A C2 H2B 108.4 . . N2 C3 C4 107.4(7) . . N2 C3 H3C 110.2 . . C4 C3 H3C 110.2 . . N2 C3 H3D 110.2 . . C4 C3 H3D 110.2 . . H3C C3 H3D 108.5 . . N3 C4 C3 109.5(7) . . N3 C4 H4C 109.8 . . C3 C4 H4C 109.8 . . N3 C4 H4D 109.8 . . C3 C4 H4D 109.8 . . H4C C4 H4D 108.2 . . N4 C5 C6 108.9(7) . . N4 C5 H5A 109.9 . . C6 C5 H5A 109.9 . . N4 C5 H5B 109.9 . . C6 C5 H5B 109.9 . . H5A C5 H5B 108.3 . . N5 C6 C5 113.4(7) . . N5 C6 H6C 108.9 . . C5 C6 H6C 108.9 . . N5 C6 H6D 108.9 . . C5 C6 H6D 108.9 . . H6C C6 H6D 107.7 . . N5 C7 C8 113.7(7) . . N5 C7 H7A 108.8 . . C8 C7 H7A 108.8 . . N5 C7 H7B 108.8 . . C8 C7 H7B 108.8 . . H7A C7 H7B 107.7 . . N6 C8 C7 111.5(7) . . N6 C8 H8A 109.3 . . C7 C8 H8A 109.3 . . N6 C8 H8B 109.3 . . C7 C8 H8B 109.3 . . H8A C8 H8B 108.0 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ge1 F1 1.807(6) . Ge1 O2 1.875(4) . Ge1 O2 1.875(4) 2_556 Ge1 O3 1.890(4) . Ge1 O3 1.890(4) 2_556 Ge1 O1 1.999(6) . Ge2 O4 1.772(4) . Ge2 O6 1.776(4) . Ge2 O5 1.785(4) . Ge2 F2 1.817(4) . Ge2 O1 1.984(4) . Ge2 Ge2 2.8472(16) 2_556 Ge3 O2 1.719(4) . Ge3 O6 1.745(5) . Ge3 O7 1.752(5) . Ge3 O8 1.754(5) . Ge4 O3 1.725(4) . Ge4 O9 1.740(2) . Ge4 O4 1.751(5) 2_556 Ge4 O8 1.754(5) . Ni1 N2 2.067(6) . Ni1 N2 2.067(6) 2_656 Ni1 N3 2.129(7) 2_656 Ni1 N3 2.129(7) . Ni1 N1 2.166(7) . Ni1 N1 2.166(7) 2_656 Ni2 N5 2.065(6) 3_666 Ni2 N5 2.065(6) . Ni2 N6 2.077(6) . Ni2 N6 2.077(6) 3_666 Ni2 N4 2.147(7) . Ni2 N4 2.147(7) 3_666 O1 Ge2 1.984(4) 2_556 O4 Ge4 1.751(5) 2_556 O5 Ge2 1.785(4) 2_556 O7 H7 0.8200 . O9 Ge4 1.740(2) 2_456 N1 C1 1.478(10) . N1 H1A 0.9000 . N1 H1B 0.9000 . N2 C3 1.466(10) . N2 C2 1.497(10) . N2 H2 0.9100 . N3 C4 1.481(10) . N3 H3A 0.9000 . N3 H3B 0.9000 . N4 C5 1.462(11) . N4 H4A 0.9000 . N4 H4B 0.9000 . N5 C6 1.449(11) . N5 C7 1.459(10) . N5 H5 0.9100 . N6 C8 1.465(10) . N6 H6A 0.9000 . N6 H6B 0.9000 . C1 C2 1.487(12) . C1 H1C 0.9700 . C1 H1D 0.9700 . C2 H2A 0.9700 . C2 H2B 0.9700 . C3 C4 1.511(12) . C3 H3C 0.9700 . C3 H3D 0.9700 . C4 H4C 0.9700 . C4 H4D 0.9700 . C5 C6 1.516(13) . C5 H5A 0.9700 . C5 H5B 0.9700 . C6 H6C 0.9700 . C6 H6D 0.9700 . C7 C8 1.467(12) . C7 H7A 0.9700 . C7 H7B 0.9700 . C8 H8A 0.9700 . C8 H8B 0.9700 . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O6 0.90 2.13 2.975(8) 155.6 3_656 N2 H2 F2 0.91 2.18 3.080(7) 170.6 . N3 H3A F2 0.90 2.32 3.165(8) 156.0 4_656 N4 H4B F1 0.90 2.14 3.008(7) 162.3 3_666 N5 H5 O3 0.91 2.42 3.311(9) 166.1 2_556 N6 H6A O2 0.90 2.06 2.885(8) 151.2 3_666