# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1929 data_volker1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C17 H35 Cl Co Ge O9 P3' _chemical_formula_sum 'C17 H35 Cl Co Ge O9 P3' _chemical_formula_weight 643.35 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.2990 0.9730 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ge' 'Ge' 0.0810 1.8010 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 12.219(3) _cell_length_b 14.260(5) _cell_length_c 15.304(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2666.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 5 _cell_measurement_theta_max 20 _exptl_crystal_description parallelepiped _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 2.010 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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-IPDS' _diffrn_measurement_method '\f-rotation' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number 200 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 27383 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 26.12 _reflns_number_total 5227 _reflns_number_gt 4593 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (STOE, 1998, Darmstadt)' _computing_cell_refinement 'IPDS (STOE, 1998, Darmdtadt)' _computing_data_reduction 'IPDS (Software 2.87, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; L.Zsolnai,H.Pritzkow, ZORTEP, ORTEP program for PC, Universit\"at Heidelberg 1994 ; _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] 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 mixed _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 -0.007(7) _refine_ls_number_reflns 5227 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0455 _refine_ls_wR_factor_gt 0.0442 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _refine_ls_shift/su_max 0.006 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.63928(3) 1.01330(2) 0.60157(2) 0.02196(8) Uani 1 d . . . C1 C 0.6778(3) 1.1470(2) 0.64804(19) 0.0449(8) Uani 1 d . . . H1 H 0.6965 1.1998 0.6133 0.054 Uiso 1 calc R . . C2 C 0.7518(3) 1.0802(2) 0.68184(19) 0.0414(8) Uani 1 d . . . H2 H 0.8288 1.0797 0.6734 0.050 Uiso 1 calc R . . C3 C 0.6907(2) 1.0142(2) 0.73050(17) 0.0354(7) Uani 1 d . . . H3 H 0.7197 0.9618 0.7610 0.042 Uiso 1 calc R . . C4 C 0.5792(2) 1.0395(2) 0.72600(17) 0.0365(7) Uani 1 d . . . H4 H 0.5198 1.0074 0.7526 0.044 Uiso 1 calc R . . C5 C 0.5724(3) 1.1218(2) 0.67447(18) 0.0409(7) Uani 1 d . . . H5 H 0.5070 1.1545 0.6603 0.049 Uiso 1 calc R . . P1 P 0.72848(6) 0.88251(5) 0.57871(4) 0.02821(15) Uani 1 d . . . O1 O 0.85398(15) 0.91222(12) 0.58413(13) 0.0395(5) Uani 1 d . . . C11 C 0.9392(3) 0.8415(2) 0.5829(3) 0.0584(10) Uani 1 d . . . H11A H 0.9191 0.7907 0.5418 0.070 Uiso 1 calc R . . H11B H 0.9475 0.8139 0.6419 0.070 Uiso 1 calc R . . C12 C 1.0426(3) 0.8846(3) 0.5556(3) 0.0677(11) Uani 1 d . . . H12A H 1.1003 0.8369 0.5546 0.102 Uiso 1 calc R . . H12B H 1.0625 0.9343 0.5968 0.102 Uiso 1 calc R . . H12C H 1.0341 0.9114 0.4970 0.102 Uiso 1 calc R . . O2 O 0.71729(18) 0.81483(13) 0.66221(13) 0.0418(5) Uani 1 d . . . C21 C 0.6519(7) 0.7265(4) 0.6620(4) 0.050(3) Uani 0.581(12) d P A 1 H21A H 0.5844 0.7358 0.6966 0.060 Uiso 0.581(12) calc PR A 1 H21B H 0.6303 0.7111 0.6013 0.060 Uiso 0.581(12) calc PR A 1 C22 C 0.7104(14) 0.6538(12) 0.6963(15) 0.110(7) Uani 0.581(12) d P A 1 H22A H 0.6653 0.5970 0.6963 0.166 Uiso 0.581(12) calc PR A 1 H22B H 0.7319 0.6690 0.7563 0.166 Uiso 0.581(12) calc PR A 1 H22C H 0.7761 0.6432 0.6609 0.166 Uiso 0.581(12) calc PR A 1 C21A C 0.7381(12) 0.7151(6) 0.6478(6) 0.066(4) Uani 0.419(12) d P A 2 H21C H 0.8170 0.7009 0.6542 0.080 Uiso 0.419(12) calc PR A 2 H21D H 0.7140 0.6960 0.5887 0.080 Uiso 0.419(12) calc PR A 2 C22A C 0.6727(19) 0.666(2) 0.717(2) 0.098(9) Uani 0.419(12) d P A 2 H22D H 0.6835 0.5978 0.7110 0.146 Uiso 0.419(12) calc PR A 2 H22E H 0.5950 0.6805 0.7090 0.146 Uiso 0.419(12) calc PR A 2 H22F H 0.6969 0.6862 0.7745 0.146 Uiso 0.419(12) calc PR A 2 O3 O 0.70397(16) 0.82764(13) 0.49813(13) 0.0373(5) Uani 1 d . . . P2 P 0.49004(5) 0.94551(5) 0.56218(4) 0.02747(16) Uani 1 d . . . O4 O 0.46242(14) 0.86720(14) 0.63196(12) 0.0388(5) Uani 1 d . . . C41 C 0.3591(3) 0.8159(2) 0.6318(2) 0.0467(8) Uani 1 d . . . H41A H 0.3737 0.7479 0.6376 0.056 Uiso 1 calc R . . H41B H 0.3206 0.8264 0.5758 0.056 Uiso 1 calc R . . C42 C 0.2889(3) 0.8478(3) 0.7053(2) 0.0554(10) Uani 1 d . . . H42A H 0.2199 0.8128 0.7046 0.083 Uiso 1 calc R . . H42B H 0.2738 0.9149 0.6990 0.083 Uiso 1 calc R . . H42C H 0.3268 0.8366 0.7608 0.083 Uiso 1 calc R . . O5 O 0.38707(14) 1.01283(15) 0.57003(12) 0.0418(5) Uani 1 d . . . C51 C 0.3220(3) 1.0413(4) 0.4987(3) 0.0873(15) Uani 1 d . . . H51A H 0.2833 0.9860 0.4746 0.105 Uiso 1 calc R . . H51B H 0.3699 1.0667 0.4522 0.105 Uiso 1 calc R . . C52 C 0.2431(3) 1.1112(4) 0.5229(3) 0.0935(16) Uani 1 d . . . H52A H 0.1998 1.1288 0.4716 0.140 Uiso 1 calc R . . H52B H 0.2811 1.1665 0.5456 0.140 Uiso 1 calc R . . H52C H 0.1946 1.0858 0.5681 0.140 Uiso 1 calc R . . O6 O 0.48303(14) 0.90233(13) 0.47085(11) 0.0325(4) Uani 1 d . . . P3 P 0.66701(5) 1.06451(5) 0.47192(4) 0.02320(15) Uani 1 d . . . O7 O 0.58039(15) 1.14449(13) 0.45222(11) 0.0310(4) Uani 1 d . . . C71 C 0.5774(3) 1.1895(2) 0.36588(19) 0.0442(7) Uani 1 d . . . H71A H 0.6384 1.2348 0.3605 0.053 Uiso 1 calc R . . H71B H 0.5855 1.1416 0.3195 0.053 Uiso 1 calc R . . C72 C 0.4725(3) 1.2381(3) 0.3561(2) 0.0742(13) Uani 1 d . . . H72A H 0.4696 1.2685 0.2987 0.111 Uiso 1 calc R . . H72B H 0.4652 1.2856 0.4020 0.111 Uiso 1 calc R . . H72C H 0.4126 1.1927 0.3609 0.111 Uiso 1 calc R . . O8 O 0.77695(14) 1.12316(13) 0.45840(12) 0.0315(4) Uani 1 d . . . C81 C 0.88330(19) 1.0793(2) 0.44829(18) 0.0316(6) Uani 1 d . . . H81A H 0.8757 1.0186 0.4175 0.038 Uiso 1 calc R . . H81B H 0.9164 1.0675 0.5063 0.038 Uiso 1 calc R . . C82 C 0.9538(2) 1.1442(2) 0.3967(2) 0.0494(8) Uani 1 d . . . H82A H 1.0265 1.1162 0.3890 0.074 Uiso 1 calc R . . H82B H 0.9609 1.2040 0.4278 0.074 Uiso 1 calc R . . H82C H 0.9206 1.1552 0.3393 0.074 Uiso 1 calc R . . O9 O 0.66603(12) 0.99381(12) 0.39638(10) 0.0275(4) Uani 1 d . . . Ge Ge 0.58404(2) 0.88118(2) 0.375982(18) 0.03110(8) Uani 1 d . . . Cl Cl 0.46542(6) 0.96685(6) 0.27776(5) 0.0503(2) Uani 1 d . . . 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 Co 0.02586(16) 0.02275(17) 0.01725(16) 0.00063(14) -0.00169(14) -0.00005(14) C1 0.077(2) 0.0289(17) 0.0291(16) -0.0082(12) 0.0006(16) -0.0102(16) C2 0.0380(16) 0.052(2) 0.0341(17) -0.0203(15) -0.0024(13) -0.0095(15) C3 0.0467(16) 0.0383(17) 0.0213(13) -0.0047(13) -0.0118(12) 0.0041(14) C4 0.0431(16) 0.0447(18) 0.0217(13) -0.0050(12) 0.0042(13) 0.0031(15) C5 0.0526(19) 0.0383(17) 0.0317(15) -0.0125(14) -0.0071(14) 0.0142(17) P1 0.0351(4) 0.0218(3) 0.0278(4) 0.0017(3) -0.0069(3) 0.0030(3) O1 0.0309(9) 0.0282(10) 0.0595(13) -0.0036(9) -0.0084(10) 0.0107(8) C11 0.0432(19) 0.0430(19) 0.089(3) -0.0051(19) -0.0165(18) 0.0175(15) C12 0.0444(19) 0.068(3) 0.091(3) -0.001(2) 0.0069(19) 0.023(2) O2 0.0614(14) 0.0263(11) 0.0377(11) 0.0072(9) -0.0104(10) -0.0015(10) C21 0.072(6) 0.035(4) 0.043(3) 0.010(3) 0.005(4) -0.019(4) C22 0.071(9) 0.043(7) 0.22(2) 0.049(11) 0.007(9) -0.011(6) C21A 0.094(10) 0.038(6) 0.067(6) 0.023(4) 0.047(6) 0.014(5) C22A 0.11(2) 0.066(11) 0.119(12) 0.018(9) 0.076(15) -0.004(12) O3 0.0514(12) 0.0274(11) 0.0331(10) -0.0070(9) -0.0124(9) 0.0084(9) P2 0.0261(3) 0.0343(4) 0.0220(4) 0.0020(3) 0.0012(3) -0.0040(3) O4 0.0329(9) 0.0480(12) 0.0354(11) 0.0131(10) 0.0014(9) -0.0150(9) C41 0.0436(16) 0.0542(19) 0.0423(18) 0.0089(15) 0.0039(16) -0.0170(15) C42 0.0481(19) 0.072(3) 0.047(2) 0.0136(18) 0.0068(16) -0.0213(18) O5 0.0328(10) 0.0563(13) 0.0362(10) -0.0009(10) -0.0020(8) 0.0081(9) C51 0.063(2) 0.130(4) 0.069(3) 0.017(3) -0.011(2) 0.048(3) C52 0.064(3) 0.086(3) 0.131(4) 0.007(3) -0.014(3) 0.030(3) O6 0.0298(9) 0.0415(12) 0.0262(10) -0.0012(8) -0.0009(8) -0.0098(8) P3 0.0256(3) 0.0234(4) 0.0206(3) 0.0015(3) 0.0003(3) -0.0008(3) O7 0.0386(10) 0.0322(11) 0.0221(9) 0.0074(7) -0.0003(9) 0.0081(9) C71 0.0602(19) 0.0407(17) 0.0317(16) 0.0168(13) -0.0021(16) 0.0048(16) C72 0.090(3) 0.084(3) 0.048(2) 0.020(2) -0.006(2) 0.049(2) O8 0.0318(9) 0.0261(10) 0.0367(10) 0.0000(9) 0.0051(8) -0.0080(8) C81 0.0249(14) 0.0382(16) 0.0317(15) 0.0004(12) 0.0016(11) -0.0006(11) C82 0.0404(16) 0.060(2) 0.0479(19) 0.0011(16) 0.0077(15) -0.0175(15) O9 0.0318(9) 0.0304(10) 0.0201(8) -0.0022(8) 0.0029(7) -0.0032(8) Ge 0.03781(15) 0.03129(16) 0.02420(14) -0.00639(13) 0.00149(13) -0.00697(14) Cl 0.0488(4) 0.0672(6) 0.0350(4) 0.0020(4) -0.0126(3) 0.0034(4) _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 Co C3 2.071(3) . ? Co C4 2.075(3) . ? Co C5 2.076(3) . ? Co C2 2.076(3) . ? Co C1 2.088(3) . ? Co P3 2.1414(8) . ? Co P2 2.1502(8) . ? Co P1 2.1884(10) . ? C1 C5 1.397(5) . ? C1 C2 1.411(4) . ? C2 C3 1.413(4) . ? C3 C4 1.412(4) . ? C4 C5 1.416(4) . ? P1 O3 1.491(2) . ? P1 O1 1.593(2) . ? P1 O2 1.607(2) . ? O1 C11 1.449(3) . ? C11 C12 1.466(5) . ? O2 C21A 1.461(9) . ? O2 C21 1.492(6) . ? C21 C22 1.36(2) . ? C21A C22A 1.50(2) . ? O3 Ge 2.4949(19) . ? P2 O6 1.5297(19) . ? P2 O4 1.5816(19) . ? P2 O5 1.5870(19) . ? O4 C41 1.459(3) . ? C41 C42 1.485(5) . ? O5 C51 1.411(4) . ? C51 C52 1.435(5) . ? O6 Ge 1.9294(18) . ? P3 O9 1.5339(18) . ? P3 O7 1.5850(19) . ? P3 O8 1.5959(18) . ? O7 C71 1.469(3) . ? C71 C72 1.464(5) . ? O8 C81 1.450(3) . ? C81 C82 1.492(4) . ? O9 Ge 1.9186(17) . ? Ge Cl 2.4193(9) . ? 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 C3 Co C4 39.81(11) . . ? C3 Co C5 66.60(12) . . ? C4 Co C5 39.91(11) . . ? C3 Co C2 39.86(12) . . ? C4 Co C2 66.95(12) . . ? C5 Co C2 66.43(13) . . ? C3 Co C1 66.52(12) . . ? C4 Co C1 66.59(12) . . ? C5 Co C1 39.21(13) . . ? C2 Co C1 39.62(13) . . ? C3 Co P3 146.39(9) . . ? C4 Co P3 147.66(9) . . ? C5 Co P3 107.82(9) . . ? C2 Co P3 106.67(9) . . ? C1 Co P3 88.20(9) . . ? C3 Co P2 121.83(9) . . ? C4 Co P2 92.20(9) . . ? C5 Co P2 98.74(9) . . ? C2 Co P2 159.11(9) . . ? C1 Co P2 134.19(10) . . ? P3 Co P2 91.59(3) . . ? C3 Co P1 90.37(9) . . ? C4 Co P1 118.47(8) . . ? C5 Co P1 156.58(8) . . ? C2 Co P1 99.00(10) . . ? C1 Co P1 136.06(11) . . ? P3 Co P1 93.65(3) . . ? P2 Co P1 89.68(3) . . ? C5 C1 C2 108.2(3) . . ? C5 C1 Co 69.92(17) . . ? C2 C1 Co 69.72(17) . . ? C1 C2 C3 107.7(3) . . ? C1 C2 Co 70.66(17) . . ? C3 C2 Co 69.88(15) . . ? C4 C3 C2 108.3(3) . . ? C4 C3 Co 70.25(15) . . ? C2 C3 Co 70.26(15) . . ? C3 C4 C5 107.2(3) . . ? C3 C4 Co 69.94(16) . . ? C5 C4 Co 70.08(16) . . ? C1 C5 C4 108.6(3) . . ? C1 C5 Co 70.87(17) . . ? C4 C5 Co 70.01(16) . . ? O3 P1 O1 112.09(11) . . ? O3 P1 O2 109.00(11) . . ? O1 P1 O2 101.54(11) . . ? O3 P1 Co 118.66(8) . . ? O1 P1 Co 104.15(7) . . ? O2 P1 Co 110.01(8) . . ? C11 O1 P1 120.37(18) . . ? O1 C11 C12 109.3(3) . . ? C21A O2 C21 43.2(5) . . ? C21A O2 P1 116.7(4) . . ? C21 O2 P1 123.4(3) . . ? C22 C21 O2 111.1(10) . . ? O2 C21A C22A 105.1(12) . . ? P1 O3 Ge 125.25(11) . . ? O6 P2 O4 108.71(11) . . ? O6 P2 O5 105.56(11) . . ? O4 P2 O5 101.93(11) . . ? O6 P2 Co 118.99(7) . . ? O4 P2 Co 108.00(8) . . ? O5 P2 Co 112.28(8) . . ? C41 O4 P2 122.54(18) . . ? O4 C41 C42 110.2(3) . . ? C51 O5 P2 124.2(2) . . ? O5 C51 C52 112.2(4) . . ? P2 O6 Ge 135.62(11) . . ? O9 P3 O7 108.93(10) . . ? O9 P3 O8 104.68(10) . . ? O7 P3 O8 99.22(11) . . ? O9 P3 Co 118.23(8) . . ? O7 P3 Co 108.42(7) . . ? O8 P3 Co 115.60(7) . . ? C71 O7 P3 120.13(18) . . ? C72 C71 O7 108.7(3) . . ? C81 O8 P3 122.81(16) . . ? O8 C81 C82 107.8(2) . . ? P3 O9 Ge 132.61(10) . . ? O9 Ge O6 94.63(7) . . ? O9 Ge Cl 89.50(6) . . ? O6 Ge Cl 90.31(6) . . ? O9 Ge O3 80.07(7) . . ? O6 Ge O3 81.94(7) . . ? Cl Ge O3 166.40(5) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.12 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.348 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.052 #============================================================================== data_peter36a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C15 H22 B Ge N15' _chemical_formula_sum 'C15 H22 B Ge N15' _chemical_formula_weight 495.90 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ge' 'Ge' 0.0810 1.8010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.378(7) _cell_length_b 10.918(13) _cell_length_c 17.719(9) _cell_angle_alpha 90.00 _cell_angle_beta 101.04(4) _cell_angle_gamma 90.00 _cell_volume 2160(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 26 _cell_measurement_theta_min 16.8 _cell_measurement_theta_max 18.2 _exptl_crystal_description parallelepiped _exptl_crystal_colour colorless _exptl_crystal_size_max 1.14 _exptl_crystal_size_mid 0.80 _exptl_crystal_size_min 0.46 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 1.403 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1926 _exptl_absorpt_correction_T_max 0.9611 _exptl_absorpt_process_details ; 6 Psi Scan Reflections used Mu * R = 0.00 H K L 2Theta Chi Imin/Imax -1 -1 1 5.9 -83.2 0.182 -2 -3 2 13.4 -84.5 0.188 -2 -3 3 14.5 -84.2 0.177 -3 -3 3 17.8 -83.2 0.201 -3 -4 3 19.3 -86.6 0.209 -4 -5 5 26.3 -87.5 0.217 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 Stadi4 Diffractometer' _diffrn_measurement_method '\w-2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 1.5 _diffrn_reflns_number 6301 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.99 _reflns_number_total 4234 _reflns_number_gt 3948 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI4 (STOE, 1995)' _computing_cell_refinement 'STADI4 (STOE, 1995)' _computing_data_reduction 'X-RED, (STOE, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1993)' _computing_molecular_graphics ; L.Zsolnai, H.Pritzkow, ZORTEP, ORTEP program for PC, Universit\"at Heidelberg 1994 ; _computing_publication_material 'SHELXL-97 (Sheldrick, 1993)' _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 w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+3.4328P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0258(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4234 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1166 _refine_ls_wR_factor_gt 0.1135 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge Ge 0.74477(2) 0.23958(2) 0.599536(15) 0.01648(14) Uani 1 d . . . B B 0.6909(3) 0.4456(3) 0.71302(16) 0.0190(6) Uani 1 d . . . H0 H 0.6733 0.5102 0.7493 0.023 Uiso 1 calc R . . N1 N 0.8179(2) 0.25665(19) 0.71296(14) 0.0196(5) Uani 1 d . . . C1 C 0.9016(2) 0.1917(3) 0.76099(15) 0.0220(6) Uani 1 d . . . C11 C 0.9536(3) 0.0730(3) 0.74168(18) 0.0290(6) Uani 1 d . . . H11A H 0.9206 0.0518 0.6881 0.044 Uiso 1 calc R . . H11B H 0.9334 0.0086 0.7756 0.044 Uiso 1 calc R . . H11C H 1.0408 0.0807 0.7487 0.044 Uiso 1 calc R . . C2 C 0.9258(3) 0.2521(3) 0.83132(17) 0.0252(6) Uani 1 d . . . H2 H 0.9816 0.2273 0.8756 0.030 Uiso 1 calc R . . C3 C 0.8540(2) 0.3543(3) 0.82501(14) 0.0223(6) Uani 1 d . . . C31 C 0.8413(3) 0.4485(3) 0.88449(15) 0.0288(6) Uani 1 d . . . H31A H 0.7821 0.5099 0.8619 0.043 Uiso 1 calc R . . H31B H 0.9187 0.4884 0.9026 0.043 Uiso 1 calc R . . H31C H 0.8147 0.4087 0.9279 0.043 Uiso 1 calc R . . N2 N 0.78838(19) 0.3565(2) 0.75293(12) 0.0194(5) Uani 1 d . . . N3 N 0.7646(2) 0.4246(2) 0.58947(12) 0.0183(5) Uani 1 d . . . C4 C 0.7987(2) 0.4950(3) 0.53475(15) 0.0219(6) Uani 1 d . . . C41 C 0.8365(3) 0.4469(3) 0.46428(16) 0.0295(6) Uani 1 d . . . H41A H 0.8332 0.3572 0.4644 0.044 Uiso 1 calc R . . H41B H 0.9185 0.4736 0.4636 0.044 Uiso 1 calc R . . H41C H 0.7825 0.4783 0.4186 0.044 Uiso 1 calc R . . C5 C 0.7914(3) 0.6171(3) 0.55525(16) 0.0243(6) Uani 1 d . . . H5 H 0.8102 0.6863 0.5273 0.029 Uiso 1 calc R . . C6 C 0.7514(2) 0.6184(2) 0.62438(15) 0.0215(5) Uani 1 d . . . C61 C 0.7277(3) 0.7244(3) 0.67267(19) 0.0326(7) Uani 1 d . . . H61A H 0.7004 0.6941 0.7185 0.049 Uiso 1 calc R . . H61B H 0.6656 0.7767 0.6429 0.049 Uiso 1 calc R . . H61C H 0.8013 0.7720 0.6883 0.049 Uiso 1 calc R . . N4 N 0.7358(2) 0.5019(2) 0.64437(12) 0.0186(5) Uani 1 d . . . N5 N 0.5864(2) 0.2746(2) 0.63110(13) 0.0200(5) Uani 1 d . . . C7 C 0.4757(3) 0.2270(3) 0.60917(17) 0.0238(6) Uani 1 d . . . C71 C 0.4464(3) 0.1215(3) 0.55542(18) 0.0317(7) Uani 1 d . . . H71A H 0.5192 0.0938 0.5386 0.048 Uiso 1 calc R . . H71B H 0.3870 0.1470 0.5106 0.048 Uiso 1 calc R . . H71C H 0.4137 0.0543 0.5817 0.048 Uiso 1 calc R . . C8 C 0.3976(3) 0.2923(3) 0.64520(17) 0.0283(6) Uani 1 d . . . H8 H 0.3141 0.2783 0.6405 0.034 Uiso 1 calc R . . C9 C 0.4644(2) 0.3817(3) 0.68925(16) 0.0249(6) Uani 1 d . . . C91 C 0.4249(3) 0.4787(3) 0.73829(19) 0.0368(7) Uani 1 d . . . H91A H 0.4942 0.5277 0.7623 0.055 Uiso 1 calc R . . H91B H 0.3887 0.4404 0.7783 0.055 Uiso 1 calc R . . H91C H 0.3659 0.5318 0.7064 0.055 Uiso 1 calc R . . N6 N 0.5786(2) 0.3695(2) 0.68076(12) 0.0203(5) Uani 1 d . . . N7 N 0.9011(2) 0.2134(2) 0.57185(14) 0.0239(5) Uani 1 d . . . N8 N 0.9894(2) 0.2637(2) 0.60760(15) 0.0247(5) Uani 1 d . . . N9 N 1.0759(3) 0.3072(3) 0.63969(18) 0.0417(7) Uani 1 d . . . N10 N 0.6691(2) 0.2257(2) 0.49208(14) 0.0255(5) Uani 1 d . . . N11 N 0.5975(2) 0.3044(3) 0.46444(14) 0.0292(6) Uani 1 d . . . N12 N 0.5304(3) 0.3754(3) 0.43498(18) 0.0503(8) Uani 1 d . . . N13 N 0.7235(2) 0.0659(2) 0.61469(14) 0.0244(5) Uani 1 d . . . N14 N 0.7821(2) -0.0028(2) 0.58189(13) 0.0222(5) Uani 1 d . . . N15 N 0.8350(2) -0.0727(2) 0.55416(15) 0.0310(6) Uani 1 d . . . 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 Ge 0.0153(2) 0.01828(19) 0.0153(2) -0.00106(9) 0.00164(12) -0.00081(9) B 0.0177(14) 0.0213(14) 0.0172(13) -0.0022(11) 0.0015(11) 0.0005(11) N1 0.0185(12) 0.0212(11) 0.0184(12) -0.0008(8) 0.0020(9) 0.0008(8) C1 0.0180(13) 0.0263(13) 0.0207(13) 0.0051(11) 0.0013(10) -0.0001(11) C11 0.0261(15) 0.0275(15) 0.0316(15) 0.0052(12) 0.0007(12) 0.0073(12) C2 0.0209(15) 0.0352(16) 0.0176(14) 0.0069(10) -0.0008(11) 0.0010(11) C3 0.0198(13) 0.0321(14) 0.0140(12) 0.0015(11) 0.0008(10) -0.0038(11) C31 0.0304(16) 0.0397(16) 0.0150(12) -0.0050(12) 0.0005(11) -0.0001(13) N2 0.0190(11) 0.0239(11) 0.0146(10) -0.0013(9) 0.0011(8) 0.0005(9) N3 0.0179(11) 0.0193(11) 0.0175(10) -0.0006(8) 0.0033(8) -0.0004(8) C4 0.0195(13) 0.0259(14) 0.0191(13) 0.0016(10) 0.0006(10) -0.0032(10) C41 0.0358(17) 0.0300(15) 0.0251(14) 0.0016(12) 0.0116(12) -0.0041(12) C5 0.0271(14) 0.0214(13) 0.0233(13) 0.0045(11) 0.0020(11) -0.0021(11) C6 0.0228(14) 0.0210(13) 0.0188(13) 0.0012(10) -0.0012(10) -0.0012(10) C61 0.047(2) 0.0228(14) 0.0284(16) -0.0055(12) 0.0079(14) -0.0018(13) N4 0.0185(11) 0.0202(11) 0.0157(10) -0.0020(8) 0.0001(8) 0.0006(8) N5 0.0166(12) 0.0240(11) 0.0185(11) -0.0026(9) 0.0013(9) -0.0016(9) C7 0.0176(14) 0.0311(15) 0.0210(14) 0.0016(11) -0.0007(11) -0.0040(11) C71 0.0237(15) 0.0373(17) 0.0325(15) -0.0072(13) 0.0015(12) -0.0108(12) C8 0.0175(14) 0.0399(16) 0.0275(15) 0.0015(13) 0.0041(11) -0.0021(12) C9 0.0203(13) 0.0337(15) 0.0215(13) 0.0033(11) 0.0061(10) 0.0039(11) C91 0.0288(16) 0.0472(19) 0.0370(17) -0.0064(15) 0.0134(13) 0.0052(14) N6 0.0189(11) 0.0246(11) 0.0171(10) -0.0010(9) 0.0025(8) 0.0001(9) N7 0.0190(12) 0.0263(12) 0.0271(12) -0.0037(10) 0.0058(10) 0.0001(10) N8 0.0207(13) 0.0254(12) 0.0290(13) 0.0054(9) 0.0073(11) 0.0009(9) N9 0.0249(15) 0.0512(18) 0.0465(17) 0.0025(14) 0.0006(13) -0.0105(13) N10 0.0261(14) 0.0306(13) 0.0184(12) -0.0041(10) 0.0006(10) -0.0027(10) N11 0.0239(13) 0.0402(15) 0.0210(12) 0.0017(11) -0.0020(10) -0.0073(12) N12 0.0350(17) 0.066(2) 0.0435(17) 0.0157(16) -0.0086(13) 0.0063(15) N13 0.0265(12) 0.0198(11) 0.0279(12) 0.0013(9) 0.0080(10) -0.0033(9) N14 0.0247(12) 0.0198(11) 0.0204(11) 0.0025(9) 0.0002(9) -0.0049(9) N15 0.0370(15) 0.0215(12) 0.0356(14) -0.0016(10) 0.0097(11) 0.0021(11) _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 Ge N13 1.937(3) . ? Ge N10 1.939(3) . ? Ge N7 1.954(3) . ? Ge N5 2.023(3) . ? Ge N1 2.031(3) . ? Ge N3 2.044(3) . ? B N4 1.535(4) . ? B N6 1.540(4) . ? B N2 1.542(4) . ? N1 C1 1.351(4) . ? N1 N2 1.376(3) . ? C1 C2 1.390(4) . ? C1 C11 1.490(4) . ? C2 C3 1.375(4) . ? C3 N2 1.351(3) . ? C3 C31 1.499(4) . ? N3 C4 1.351(4) . ? N3 N4 1.374(3) . ? C4 C5 1.388(4) . ? C4 C41 1.492(4) . ? C5 C6 1.386(4) . ? C6 N4 1.341(4) . ? C6 C61 1.494(4) . ? N5 C7 1.349(4) . ? N5 N6 1.373(3) . ? C7 C8 1.387(4) . ? C7 C71 1.492(4) . ? C8 C9 1.383(4) . ? C9 N6 1.343(4) . ? C9 C91 1.493(4) . ? N7 N8 1.212(4) . ? N8 N9 1.142(4) . ? N10 N11 1.220(4) . ? N11 N12 1.141(4) . ? N13 N14 1.221(4) . ? N14 N15 1.141(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 N13 Ge N10 90.91(11) . . ? N13 Ge N7 92.04(11) . . ? N10 Ge N7 89.79(12) . . ? N13 Ge N5 90.29(10) . . ? N10 Ge N5 91.99(11) . . ? N7 Ge N5 177.05(9) . . ? N13 Ge N1 89.49(10) . . ? N10 Ge N1 177.78(10) . . ? N7 Ge N1 92.38(11) . . ? N5 Ge N1 85.82(11) . . ? N13 Ge N3 176.75(9) . . ? N10 Ge N3 91.55(10) . . ? N7 Ge N3 90.09(10) . . ? N5 Ge N3 87.51(10) . . ? N1 Ge N3 87.97(9) . . ? N4 B N6 107.5(2) . . ? N4 B N2 107.3(2) . . ? N6 B N2 107.6(2) . . ? C1 N1 N2 107.7(2) . . ? C1 N1 Ge 132.9(2) . . ? N2 N1 Ge 119.19(17) . . ? N1 C1 C2 108.1(3) . . ? N1 C1 C11 125.1(2) . . ? C2 C1 C11 126.8(3) . . ? C3 C2 C1 107.5(3) . . ? N2 C3 C2 107.6(2) . . ? N2 C3 C31 122.9(3) . . ? C2 C3 C31 129.5(3) . . ? C3 N2 N1 109.1(2) . . ? C3 N2 B 131.6(2) . . ? N1 N2 B 119.3(2) . . ? C4 N3 N4 107.4(2) . . ? C4 N3 Ge 132.56(19) . . ? N4 N3 Ge 120.03(17) . . ? N3 C4 C5 108.6(2) . . ? N3 C4 C41 124.7(3) . . ? C5 C4 C41 126.7(3) . . ? C6 C5 C4 106.7(2) . . ? N4 C6 C5 107.8(2) . . ? N4 C6 C61 122.4(3) . . ? C5 C6 C61 129.8(3) . . ? C6 N4 N3 109.5(2) . . ? C6 N4 B 132.1(2) . . ? N3 N4 B 118.4(2) . . ? C7 N5 N6 107.7(2) . . ? C7 N5 Ge 132.8(2) . . ? N6 N5 Ge 119.33(17) . . ? N5 C7 C8 108.4(3) . . ? N5 C7 C71 124.3(3) . . ? C8 C7 C71 127.3(3) . . ? C9 C8 C7 106.9(3) . . ? N6 C9 C8 107.8(3) . . ? N6 C9 C91 122.8(3) . . ? C8 C9 C91 129.4(3) . . ? C9 N6 N5 109.3(2) . . ? C9 N6 B 131.0(2) . . ? N5 N6 B 119.6(2) . . ? N8 N7 Ge 120.4(2) . . ? N9 N8 N7 176.7(3) . . ? N11 N10 Ge 118.4(2) . . ? N12 N11 N10 176.5(3) . . ? N14 N13 Ge 116.1(2) . . ? N15 N14 N13 175.6(3) . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.673 _refine_diff_density_min -0.876 _refine_diff_density_rms 0.099 #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author ; Alexander C. Filippou Institut f\"ur Anorganische und Allgemeine Chemie der Humboldt Universit\"at zu Berlin Hessische Strasse 1-2 10115 Berlin Bundesrepublik Deutschland ; _publ_contact_author_phone '# 49 30 2093-7385' _publ_contact_author_fax '# 49 30 2093-6939' _publ_contact_author_email 'filippou@chemie.hu-berlin.de' _publ_requested_journal 'J. Chem. Soc. Dalton Trans.' _publ_requested_coeditor_name ; Peter Portius, Gabriele Kociok-K\"ohn and Volker Albrecht ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Oxidation of azidogermylenes with HN3: A convenient route to hexacoordinate triazidogermanes ; loop_ _publ_author_name _publ_author_address 'Alexander C. Filippou' ; Institut f\"ur Anorganische und Allgemeine Chemie der Humboldt Universit\"at zu Berlin Hessische Strasse 1-2 10115 Berlin Bundesrepublik Deutschland ; 'Peter Portius' ; Institut f\"ur Anorganische und Allgemeine Chemie der Humboldt Universit\"at zu Berlin Hessische Strasse 1-2 10115 Berlin Bundesrepublik Deutschland ; 'Gabriele Kociok-K\"ohn' ; Institut f\"ur Anorganische und Allgemeine Chemie der Humboldt Universit\"at zu Berlin Hessische Strasse 1-2 10115 Berlin Bundesrepublik Deutschland ; 'Volker Albrecht' ; Institut f\"ur Anorganische und Allgemeine Chemie der Humboldt Universit\"at zu Berlin Hessische Strasse 1-2 10115 Berlin Bundesrepublik Deutschland ; #============================================================================== data_peter42 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C17 H35 Co Ge N3 O9 P3' _chemical_formula_sum 'C17 H35 Co Ge N3 O9 P3' _chemical_formula_weight 649.93 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ge' 'Ge' 0.0810 1.8010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.2990 0.9730 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.4580(12) _cell_length_b 17.226(2) _cell_length_c 18.673(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.29(2) _cell_angle_gamma 90.00 _cell_volume 2716.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 3056 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 26.09 _exptl_crystal_description 'irregular shape' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 1.882 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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-IPDS' _diffrn_measurement_method '\f-oscillation' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number 200 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 7342 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0923 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 26.09 _reflns_number_total 4391 _reflns_number_gt 2603 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (STOE, 1998, Darmstadt)' _computing_cell_refinement 'IPDS (STOE, 1998, Darmdtadt)' _computing_data_reduction 'IPDS (Software 2.87, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; L.Zsolnai,H.Pritzkow, ZORTEP, ORTEP program for PC, Universit\"at Heidelberg 1994 ; _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4391 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0897 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.0950 _refine_ls_wR_factor_gt 0.0845 _refine_ls_goodness_of_fit_ref 0.878 _refine_ls_restrained_S_all 0.878 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.13598(5) 0.05771(3) 0.20498(4) 0.02586(17) Uani 1 d . . . C1 C 0.3726(5) 0.0830(3) 0.1862(4) 0.0434(16) Uani 1 d . . . H1 H 0.4334 0.1249 0.2062 0.052 Uiso 1 calc R . . C2 C 0.2790(6) 0.0863(3) 0.1219(4) 0.0493(17) Uani 1 d . . . H2 H 0.2628 0.1303 0.0917 0.059 Uiso 1 calc R . . C3 C 0.2136(5) 0.0118(3) 0.1106(4) 0.0499(17) Uani 1 d . . . H3 H 0.1478 -0.0040 0.0703 0.060 Uiso 1 calc R . . C4 C 0.2632(5) -0.0353(3) 0.1697(4) 0.0462(17) Uani 1 d . . . H4 H 0.2342 -0.0879 0.1768 0.055 Uiso 1 calc R . . C5 C 0.3635(5) 0.0098(3) 0.2165(4) 0.0447(15) Uani 1 d . . . H5 H 0.4149 -0.0070 0.2604 0.054 Uiso 1 calc R . . P1 P -0.10578(12) 0.04952(7) 0.15686(8) 0.0355(3) Uani 1 d . . . O1 O -0.1140(3) 0.0788(2) 0.0753(2) 0.0471(10) Uani 1 d . . . C11 C -0.1768(6) 0.1546(4) 0.0559(5) 0.071(2) Uani 1 d . . . H11A H -0.1083 0.1799 0.0215 0.085 Uiso 1 calc R . . H11B H -0.1784 0.1878 0.0992 0.085 Uiso 1 calc R . . C12 C -0.3404(6) 0.1462(4) 0.0229(5) 0.077(2) Uani 1 d . . . H12A H -0.3837 0.1976 0.0108 0.116 Uiso 1 calc R . . H12B H -0.4074 0.1207 0.0570 0.116 Uiso 1 calc R . . H12C H -0.3377 0.1148 -0.0207 0.116 Uiso 1 calc R . . O2 O -0.1344(4) -0.0401(2) 0.1446(3) 0.0565(12) Uani 1 d . . . C21 C -0.2847(8) -0.0647(4) 0.1091(6) 0.102(3) Uani 1 d . . . H21A H -0.3674 -0.0260 0.1184 0.123 Uiso 1 calc R . . H21B H -0.2736 -0.0669 0.0566 0.123 Uiso 1 calc R . . C22 C -0.3311(7) -0.1360(4) 0.1327(5) 0.089(3) Uani 1 d . . . H22A H -0.4317 -0.1505 0.1076 0.134 Uiso 1 calc R . . H22B H -0.3446 -0.1337 0.1844 0.134 Uiso 1 calc R . . H22C H -0.2502 -0.1747 0.1228 0.134 Uiso 1 calc R . . O3 O -0.2352(3) 0.0878(2) 0.1947(3) 0.0602(13) Uani 1 d . . . P2 P 0.06539(12) 0.00588(6) 0.30265(8) 0.0303(3) Uani 1 d . . . O4 O 0.0645(3) -0.08604(16) 0.3019(2) 0.0414(10) Uani 1 d . . . C41 C -0.0684(7) -0.1337(3) 0.3020(6) 0.099(4) Uani 1 d . . . H41A H -0.1456 -0.1095 0.3330 0.119 Uiso 1 calc R . . H41B H -0.1179 -0.1353 0.2527 0.119 Uiso 1 calc R . . C42 C -0.0434(7) -0.2095(3) 0.3250(5) 0.086(3) Uani 1 d . . . H42A H -0.1447 -0.2373 0.3234 0.129 Uiso 1 calc R . . H42B H 0.0032 -0.2094 0.3742 0.129 Uiso 1 calc R . . H42C H 0.0288 -0.2355 0.2934 0.129 Uiso 1 calc R . . O5 O 0.1979(3) 0.02274(19) 0.3641(2) 0.0441(10) Uani 1 d . . . C51 C 0.1776(6) -0.0080(4) 0.4353(4) 0.0578(17) Uani 1 d . . . H51A H 0.2140 -0.0626 0.4377 0.069 Uiso 1 calc R . . H51B H 0.0641 -0.0069 0.4455 0.069 Uiso 1 calc R . . C52 C 0.2705(8) 0.0392(4) 0.4902(5) 0.086(2) Uani 1 d . . . H52A H 0.2559 0.0179 0.5380 0.129 Uiso 1 calc R . . H52B H 0.2334 0.0931 0.4881 0.129 Uiso 1 calc R . . H52C H 0.3830 0.0374 0.4804 0.129 Uiso 1 calc R . . O6 O -0.0964(3) 0.02879(17) 0.3309(2) 0.0425(10) Uani 1 d . . . P3 P 0.09155(12) 0.17268(6) 0.24343(8) 0.0308(3) Uani 1 d . . . O7 O 0.2409(3) 0.21349(19) 0.2838(3) 0.0444(10) Uani 1 d . . . C71 C 0.2810(11) 0.2049(5) 0.3561(6) 0.126(4) Uani 1 d . . . H71A H 0.2942 0.1488 0.3661 0.151 Uiso 1 calc R . . H71B H 0.1906 0.2231 0.3830 0.151 Uiso 1 calc R . . C72 C 0.4169(7) 0.2430(5) 0.3836(5) 0.102(3) Uani 1 d . . . H72A H 0.4323 0.2323 0.4351 0.152 Uiso 1 calc R . . H72B H 0.4048 0.2990 0.3761 0.152 Uiso 1 calc R . . H72C H 0.5090 0.2244 0.3590 0.152 Uiso 1 calc R . . O8 O 0.0656(3) 0.22881(16) 0.1771(2) 0.0379(10) Uani 1 d . . . C81 C 0.0563(6) 0.3126(3) 0.1872(4) 0.0559(18) Uani 1 d . . . H81A H 0.1635 0.3339 0.1986 0.067 Uiso 1 calc R . . H81B H -0.0103 0.3244 0.2277 0.067 Uiso 1 calc R . . C82 C -0.0131(6) 0.3489(3) 0.1209(5) 0.064(2) Uani 1 d . . . H82A H -0.0202 0.4052 0.1277 0.096 Uiso 1 calc R . . H82B H -0.1192 0.3277 0.1099 0.096 Uiso 1 calc R . . H82C H 0.0543 0.3379 0.0811 0.096 Uiso 1 calc R . . O9 O -0.0446(3) 0.18467(17) 0.2936(2) 0.0422(10) Uani 1 d . . . Ge Ge -0.21153(5) 0.12390(3) 0.32832(4) 0.04584(19) Uani 1 d . . . N1 N -0.1136(6) 0.1451(3) 0.4320(4) 0.0692(18) Uani 1 d . . . N2 N -0.1745(5) 0.1900(3) 0.4694(3) 0.0579(15) Uani 1 d . . . N3 N -0.2305(7) 0.2331(4) 0.5083(5) 0.092(2) Uani 1 d . . . 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 Co 0.0237(2) 0.0257(3) 0.0286(5) -0.0007(3) 0.0060(2) 0.0005(2) C1 0.028(2) 0.047(3) 0.057(5) -0.005(3) 0.015(2) -0.003(2) C2 0.045(3) 0.054(3) 0.051(5) 0.017(3) 0.031(3) 0.015(2) C3 0.040(2) 0.072(4) 0.039(5) -0.030(3) 0.013(2) 0.005(3) C4 0.044(2) 0.036(3) 0.061(6) -0.005(3) 0.023(3) 0.009(2) C5 0.029(2) 0.055(3) 0.051(5) 0.002(3) 0.005(2) 0.015(2) P1 0.0277(5) 0.0478(7) 0.0309(10) 0.0003(7) 0.0011(5) -0.0032(5) O1 0.0420(16) 0.060(2) 0.039(3) 0.010(2) -0.0020(15) 0.0067(15) C11 0.079(4) 0.066(4) 0.063(7) 0.012(4) -0.022(4) 0.007(3) C12 0.067(4) 0.113(6) 0.050(7) -0.022(4) -0.016(3) 0.040(3) O2 0.0547(19) 0.051(2) 0.062(4) 0.010(2) -0.0178(19) -0.0177(16) C21 0.090(5) 0.095(6) 0.116(11) 0.021(6) -0.043(5) -0.056(4) C22 0.075(4) 0.085(5) 0.103(9) 0.019(5) -0.041(4) -0.035(3) O3 0.0247(15) 0.105(3) 0.051(4) -0.007(2) 0.0030(16) 0.0105(16) P2 0.0320(5) 0.0293(6) 0.0301(10) 0.0029(6) 0.0069(5) 0.0016(5) O4 0.0482(16) 0.0256(15) 0.052(3) 0.0029(17) 0.0122(17) -0.0010(13) C41 0.072(4) 0.044(4) 0.177(12) 0.038(5) -0.024(5) -0.025(3) C42 0.075(4) 0.042(3) 0.141(10) 0.024(4) 0.022(4) -0.007(3) O5 0.0480(17) 0.048(2) 0.036(3) 0.0062(18) 0.0004(16) -0.0042(15) C51 0.071(3) 0.068(4) 0.035(5) 0.013(3) 0.007(3) 0.003(3) C52 0.107(5) 0.101(6) 0.048(8) 0.007(5) -0.021(4) -0.023(4) O6 0.0394(15) 0.0439(18) 0.046(3) 0.0138(18) 0.0197(17) 0.0125(13) P3 0.0363(5) 0.0283(6) 0.0278(10) 0.0006(6) 0.0027(5) 0.0024(5) O7 0.0473(17) 0.045(2) 0.040(3) -0.0054(19) -0.0067(16) -0.0059(14) C71 0.192(8) 0.123(7) 0.056(9) 0.027(6) -0.048(6) -0.112(6) C72 0.082(4) 0.149(7) 0.069(9) -0.050(6) -0.032(4) 0.033(4) O8 0.0492(16) 0.0265(16) 0.038(3) 0.0068(16) 0.0017(16) -0.0018(13) C81 0.070(3) 0.029(3) 0.069(6) 0.001(3) 0.001(3) 0.008(2) C82 0.077(4) 0.036(3) 0.078(7) 0.018(3) -0.005(3) 0.010(3) O9 0.0546(17) 0.0329(17) 0.041(3) -0.0019(17) 0.0191(17) 0.0100(14) Ge 0.0391(3) 0.0560(4) 0.0441(5) 0.0079(3) 0.0170(2) 0.0177(2) N1 0.085(3) 0.086(4) 0.039(5) 0.006(3) 0.020(3) 0.037(3) N2 0.057(3) 0.076(3) 0.041(5) 0.006(3) 0.008(3) 0.000(3) N3 0.111(4) 0.100(5) 0.067(7) -0.036(4) 0.006(4) 0.021(4) _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 Co C4 2.059(4) . ? Co C3 2.072(6) . ? Co C2 2.080(5) . ? Co C5 2.094(4) . ? Co C1 2.097(4) . ? Co P2 2.1459(16) . ? Co P3 2.1471(13) . ? Co P1 2.1904(13) . ? C1 C5 1.386(7) . ? C1 C2 1.401(9) . ? C2 C3 1.408(7) . ? C3 C4 1.414(9) . ? C4 C5 1.414(8) . ? P1 O3 1.490(4) . ? P1 O2 1.577(4) . ? P1 O1 1.602(5) . ? O1 C11 1.448(6) . ? C11 C12 1.489(8) . ? O2 C21 1.462(7) . ? C21 C22 1.369(9) . ? O3 Ge 2.567(5) . ? P2 O6 1.545(3) . ? P2 O4 1.583(3) . ? P2 O5 1.584(4) . ? O4 C41 1.393(6) . ? C41 C42 1.386(7) . ? O5 C51 1.450(8) . ? C51 C52 1.495(10) . ? O6 Ge 1.905(3) . ? P3 O9 1.539(3) . ? P3 O8 1.577(4) . ? P3 O7 1.597(4) . ? O7 C71 1.380(11) . ? C71 C72 1.396(9) . ? O8 C81 1.459(5) . ? C81 C82 1.477(10) . ? O9 Ge 1.901(3) . ? Ge N1 2.094(7) . ? N1 N2 1.180(7) . ? N2 N3 1.159(8) . ? 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 C4 Co C3 40.0(2) . . ? C4 Co C2 66.9(2) . . ? C3 Co C2 39.6(2) . . ? C4 Co C5 39.8(2) . . ? C3 Co C5 66.6(2) . . ? C2 Co C5 66.4(2) . . ? C4 Co C1 65.60(19) . . ? C3 Co C1 65.5(2) . . ? C2 Co C1 39.2(2) . . ? C5 Co C1 38.63(19) . . ? C4 Co P2 97.13(19) . . ? C3 Co P2 132.94(18) . . ? C2 Co P2 159.10(16) . . ? C5 Co P2 92.71(17) . . ? C1 Co P2 122.88(19) . . ? C4 Co P3 158.33(14) . . ? C3 Co P3 134.94(18) . . ? C2 Co P3 98.72(15) . . ? C5 Co P3 120.46(15) . . ? C1 Co P3 92.93(14) . . ? P2 Co P3 92.12(5) . . ? C4 Co P1 108.15(18) . . ? C3 Co P1 87.73(15) . . ? C2 Co P1 106.17(19) . . ? C5 Co P1 147.96(16) . . ? C1 Co P1 145.3(2) . . ? P2 Co P1 91.33(5) . . ? P3 Co P1 91.11(5) . . ? C5 C1 C2 110.1(5) . . ? C5 C1 Co 70.6(2) . . ? C2 C1 Co 69.7(3) . . ? C1 C2 C3 106.9(5) . . ? C1 C2 Co 71.1(3) . . ? C3 C2 Co 69.9(3) . . ? C2 C3 C4 108.0(5) . . ? C2 C3 Co 70.5(3) . . ? C4 C3 Co 69.5(3) . . ? C3 C4 C5 108.0(5) . . ? C3 C4 Co 70.5(3) . . ? C5 C4 Co 71.4(3) . . ? C1 C5 C4 107.0(6) . . ? C1 C5 Co 70.8(2) . . ? C4 C5 Co 68.7(2) . . ? O3 P1 O2 113.0(2) . . ? O3 P1 O1 108.6(2) . . ? O2 P1 O1 99.9(2) . . ? O3 P1 Co 118.06(18) . . ? O2 P1 Co 104.75(14) . . ? O1 P1 Co 111.00(12) . . ? C11 O1 P1 121.1(4) . . ? O1 C11 C12 109.5(5) . . ? C21 O2 P1 118.2(4) . . ? C22 C21 O2 111.9(7) . . ? P1 O3 Ge 123.4(2) . . ? O6 P2 O4 104.75(16) . . ? O6 P2 O5 108.0(2) . . ? O4 P2 O5 101.1(2) . . ? O6 P2 Co 118.58(15) . . ? O4 P2 Co 114.19(16) . . ? O5 P2 Co 108.64(14) . . ? C41 O4 P2 126.4(3) . . ? C42 C41 O4 116.6(5) . . ? C51 O5 P2 118.8(3) . . ? O5 C51 C52 110.2(5) . . ? P2 O6 Ge 132.27(19) . . ? O9 P3 O8 108.69(18) . . ? O9 P3 O7 104.6(2) . . ? O8 P3 O7 99.89(19) . . ? O9 P3 Co 118.59(13) . . ? O8 P3 Co 108.79(15) . . ? O7 P3 Co 114.54(13) . . ? C71 O7 P3 124.0(4) . . ? O7 C71 C72 117.5(8) . . ? C81 O8 P3 120.8(4) . . ? O8 C81 C82 109.4(6) . . ? P3 O9 Ge 136.9(2) . . ? O9 Ge O6 95.36(12) . . ? O9 Ge N1 87.56(19) . . ? O6 Ge N1 87.25(19) . . ? O9 Ge O3 79.62(15) . . ? O6 Ge O3 80.04(16) . . ? N1 Ge O3 160.95(14) . . ? N2 N1 Ge 119.9(5) . . ? N3 N2 N1 177.4(8) . . ? _diffrn_measured_fraction_theta_max 0.787 _diffrn_reflns_theta_full 26.09 _diffrn_measured_fraction_theta_full 0.787 _refine_diff_density_max 0.512 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.070 #============================================================================== data_peter48 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H35 Co Ge N9 O9 P3' _chemical_formula_weight 733.97 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' 'P' 'P' 0.1023 0.0942 '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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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' _cell_length_a 17.1284(14) _cell_length_b 12.0633(10) _cell_length_c 14.6659(8) _cell_angle_alpha 90.00 _cell_angle_beta 97.283(8) _cell_angle_gamma 90.00 _cell_volume 3005.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.622 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 1.771 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 7938 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.05 _reflns_number_total 5339 _reflns_number_gt 4965 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0776P)^2^+9.5651P] 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 mixed _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 0.021(17) _refine_ls_number_reflns 5339 _refine_ls_number_parameters 371 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1411 _refine_ls_wR_factor_gt 0.1360 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.29617(4) 0.78975(6) 0.73908(5) 0.0408(2) Uani 1 d . . . C1 C 0.3176(5) 0.8590(6) 0.8702(4) 0.0594(17) Uani 1 d . . . H1 H 0.3550 0.9150 0.8894 0.071 Uiso 1 calc R . . C2 C 0.3296(5) 0.7417(8) 0.8738(5) 0.0657(19) Uani 1 d . . . H2 H 0.3775 0.7050 0.8954 0.079 Uiso 1 calc R . . C3 C 0.2584(6) 0.6904(9) 0.8400(6) 0.075(3) Uani 1 d . . . H3 H 0.2500 0.6127 0.8350 0.090 Uiso 1 calc R . . C4 C 0.2019(6) 0.7713(9) 0.8147(6) 0.077(3) Uani 1 d . . . H4 H 0.1487 0.7583 0.7902 0.093 Uiso 1 calc R . . C5 C 0.2369(5) 0.8743(9) 0.8315(5) 0.078(3) Uani 1 d . . . H5 H 0.2116 0.9438 0.8193 0.093 Uiso 1 calc R . . P1 P 0.29121(11) 0.93417(13) 0.65302(12) 0.0464(4) Uani 1 d . . . O1 O 0.2029(3) 0.9724(4) 0.6283(4) 0.0649(13) Uani 1 d . . . C11 C 0.1818(7) 1.0618(10) 0.5635(9) 0.105(4) Uani 1 d . . . H11A H 0.2141 1.1276 0.5835 0.126 Uiso 1 calc R . . H11B H 0.1955 1.0391 0.5026 0.126 Uiso 1 calc R . . C12 C 0.1043(11) 1.0915(13) 0.5539(13) 0.168(8) Uani 1 d . . . H12A H 0.0953 1.1524 0.5096 0.252 Uiso 1 calc R . . H12B H 0.0901 1.1156 0.6135 0.252 Uiso 1 calc R . . H12C H 0.0717 1.0279 0.5318 0.252 Uiso 1 calc R . . O2 O 0.3271(4) 1.0430(6) 0.7024(4) 0.0873(19) Uani 1 d . . . C21 C 0.370(2) 1.1135(19) 0.652(3) 0.098(11) Uani 0.39(3) d P A 1 H21A H 0.4071 1.0674 0.6219 0.118 Uiso 0.39(3) calc PR A 1 H21B H 0.3323 1.1461 0.6017 0.118 Uiso 0.39(3) calc PR A 1 C21A C 0.4010(9) 1.0858(14) 0.7177(14) 0.072(7) Uani 0.61(3) d P A 2 H21C H 0.4356 1.0405 0.6833 0.087 Uiso 0.61(3) calc PR A 2 H21D H 0.4203 1.0777 0.7839 0.087 Uiso 0.61(3) calc PR A 2 C22 C 0.4092(9) 1.1944(10) 0.6940(12) 0.122(5) Uani 1 d . . . H22A H 0.4355 1.2371 0.6499 0.183 Uiso 1 calc R B 1 H22B H 0.4487 1.1642 0.7417 0.183 Uiso 1 calc R B 1 H22C H 0.3732 1.2429 0.7224 0.183 Uiso 1 calc R B 1 O3 O 0.3276(4) 0.9244(5) 0.5646(4) 0.0820(19) Uani 1 d . . . P2 P 0.41241(10) 0.75526(15) 0.70558(12) 0.0472(4) Uani 1 d . . . O4 O 0.4703(3) 0.8478(6) 0.7488(4) 0.0785(17) Uani 1 d . . . C41 C 0.5482(6) 0.8633(12) 0.7223(9) 0.117(5) Uani 1 d . . . H41A H 0.5440 0.8763 0.6552 0.140 Uiso 1 calc R . . H41B H 0.5799 0.7954 0.7366 0.140 Uiso 1 calc R . . C42 C 0.5874(6) 0.9575(10) 0.7710(10) 0.109(4) Uani 1 d . . . H42A H 0.6401 0.9664 0.7525 0.163 Uiso 1 calc R . . H42B H 0.5919 0.9443 0.8374 0.163 Uiso 1 calc R . . H42C H 0.5566 1.0249 0.7557 0.163 Uiso 1 calc R . . O5 O 0.4528(4) 0.6492(5) 0.7547(4) 0.0777(16) Uani 1 d . . . C51 C 0.4419(5) 0.5402(9) 0.7311(7) 0.084(3) Uani 1 d . . . H51A H 0.4351 0.5326 0.6633 0.101 Uiso 1 calc R . . H51B H 0.3938 0.5119 0.7541 0.101 Uiso 1 calc R . . C52 C 0.5127(6) 0.4736(8) 0.7724(8) 0.093(3) Uani 1 d . . . H52A H 0.5050 0.3954 0.7554 0.139 Uiso 1 calc R . . H52B H 0.5188 0.4807 0.8395 0.139 Uiso 1 calc R . . H52C H 0.5600 0.5016 0.7490 0.139 Uiso 1 calc R . . O6 O 0.4216(3) 0.7465(5) 0.6021(3) 0.0567(11) Uani 1 d . . . P3 P 0.24284(10) 0.69482(14) 0.62324(12) 0.0473(4) Uani 1 d . . . O7 O 0.2510(4) 0.5692(5) 0.6445(4) 0.0819(17) Uani 1 d . . . C71 C 0.2199(9) 0.4864(9) 0.5695(8) 0.114(4) Uani 1 d . . . H71A H 0.1617 0.4846 0.5637 0.136 Uiso 1 calc R . . H71B H 0.2353 0.5110 0.5099 0.136 Uiso 1 calc R . . C72 C 0.2488(9) 0.3824(8) 0.5892(9) 0.113(4) Uani 1 d . . . H72A H 0.2272 0.3311 0.5406 0.170 Uiso 1 calc R . . H72B H 0.2335 0.3579 0.6481 0.170 Uiso 1 calc R . . H72C H 0.3063 0.3835 0.5929 0.170 Uiso 1 calc R . . O8 O 0.1508(3) 0.7116(5) 0.6052(4) 0.0678(14) Uani 1 d . . . C81 C 0.1045(9) 0.7524(16) 0.5271(15) 0.171(9) Uani 1 d . . . H81A H 0.0917 0.8305 0.5396 0.206 Uiso 1 calc R . . H81B H 0.1376 0.7532 0.4764 0.206 Uiso 1 calc R . . C82 C 0.0389(10) 0.7029(18) 0.4966(14) 0.174(9) Uani 1 d . . . H82A H 0.0133 0.7423 0.4425 0.261 Uiso 1 calc R . . H82B H 0.0040 0.7026 0.5446 0.261 Uiso 1 calc R . . H82C H 0.0499 0.6264 0.4797 0.261 Uiso 1 calc R . . O9 O 0.2733(4) 0.7187(5) 0.5295(4) 0.0756(17) Uani 1 d . . . Ge Ge 0.35988(4) 0.80341(7) 0.49711(4) 0.0580(2) Uani 1 d . . . N1 N 0.4446(5) 0.8978(6) 0.4679(5) 0.083(2) Uani 1 d . . . N2 N 0.5033(5) 0.8609(6) 0.4487(5) 0.0703(18) Uani 1 d . . . N3 N 0.5590(6) 0.8343(9) 0.4270(12) 0.147(5) Uani 1 d . . . N4 N 0.3928(6) 0.6828(6) 0.4248(6) 0.087(3) Uani 1 d . . . N5 N 0.3960(5) 0.5925(6) 0.4528(5) 0.076(2) Uani 1 d . . . N6 N 0.4007(7) 0.5017(9) 0.4766(7) 0.114(3) Uani 1 d . . . N7 N 0.2912(7) 0.8699(9) 0.3945(6) 0.101(3) Uani 1 d . . . N8 N 0.2499(7) 0.8121(10) 0.3467(7) 0.109(3) Uani 1 d . . . N9 N 0.2144(10) 0.7615(15) 0.2928(10) 0.164(6) Uani 1 d . . . 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 Co 0.0399(4) 0.0508(4) 0.0317(4) 0.0044(3) 0.0050(3) -0.0019(4) C1 0.083(5) 0.067(4) 0.029(3) 0.003(3) 0.011(3) -0.006(4) C2 0.075(5) 0.084(5) 0.037(4) 0.017(4) 0.003(3) 0.012(4) C3 0.099(7) 0.089(6) 0.040(4) 0.006(4) 0.017(4) -0.036(5) C4 0.065(5) 0.118(8) 0.051(4) -0.001(5) 0.013(4) -0.028(5) C5 0.084(5) 0.119(7) 0.035(3) 0.017(4) 0.026(4) 0.046(6) P1 0.0553(9) 0.0457(8) 0.0403(8) 0.0041(7) 0.0143(7) 0.0028(7) O1 0.067(3) 0.065(3) 0.065(3) 0.028(3) 0.018(2) 0.020(2) C11 0.122(9) 0.086(7) 0.110(8) 0.046(6) 0.032(7) 0.038(6) C12 0.194(17) 0.113(11) 0.174(15) 0.034(11) -0.062(13) 0.062(11) O2 0.111(5) 0.085(4) 0.066(4) 0.000(3) 0.011(3) -0.039(4) C21 0.17(3) 0.050(12) 0.08(2) 0.020(12) 0.03(2) -0.022(15) C21A 0.068(9) 0.070(9) 0.081(13) -0.030(9) 0.021(8) -0.039(7) C22 0.139(11) 0.083(7) 0.157(13) -0.005(8) 0.064(10) -0.016(7) O3 0.131(5) 0.068(3) 0.058(3) 0.027(3) 0.054(3) 0.029(3) P2 0.0410(8) 0.0567(9) 0.0435(8) -0.0032(7) 0.0035(6) 0.0011(7) O4 0.054(3) 0.108(4) 0.076(4) -0.039(3) 0.020(3) -0.017(3) C41 0.062(5) 0.155(11) 0.140(10) -0.092(9) 0.041(6) -0.042(6) C42 0.068(5) 0.108(8) 0.150(11) -0.047(8) 0.008(6) -0.032(5) O5 0.087(4) 0.083(4) 0.061(3) -0.001(3) 0.003(3) 0.033(3) C51 0.069(5) 0.103(7) 0.079(6) 0.008(5) 0.005(4) -0.005(5) C52 0.077(6) 0.077(6) 0.120(8) 0.032(6) -0.007(5) 0.013(5) O6 0.054(3) 0.069(3) 0.050(3) -0.001(2) 0.015(2) 0.010(2) P3 0.0450(8) 0.0504(9) 0.0453(9) -0.0003(7) 0.0006(7) -0.0068(7) O7 0.100(4) 0.060(3) 0.077(4) -0.005(3) -0.023(3) -0.003(3) C71 0.159(11) 0.078(7) 0.096(8) -0.001(6) -0.015(7) -0.035(7) C72 0.170(12) 0.055(5) 0.122(9) -0.022(6) 0.044(8) -0.028(6) O8 0.054(3) 0.082(4) 0.065(3) 0.001(3) -0.004(2) 0.000(3) C81 0.098(9) 0.188(16) 0.200(17) 0.077(14) -0.093(11) -0.029(10) C82 0.117(11) 0.25(2) 0.136(13) -0.011(13) -0.062(10) 0.020(12) O9 0.084(4) 0.097(4) 0.045(3) -0.017(3) 0.007(3) -0.041(3) Ge 0.0703(5) 0.0661(5) 0.0406(4) -0.0026(3) 0.0194(3) 0.0004(4) N1 0.116(6) 0.069(4) 0.074(5) -0.002(4) 0.051(4) -0.003(4) N2 0.078(5) 0.068(4) 0.070(4) 0.021(3) 0.027(4) 0.013(4) N3 0.092(7) 0.103(7) 0.256(16) 0.086(9) 0.071(9) 0.026(6) N4 0.147(8) 0.056(4) 0.067(5) -0.026(4) 0.054(5) -0.015(4) N5 0.111(6) 0.059(4) 0.065(4) -0.025(3) 0.038(4) -0.020(4) N6 0.168(10) 0.081(6) 0.103(7) -0.030(5) 0.057(7) -0.007(6) N7 0.132(8) 0.113(7) 0.059(5) 0.026(5) 0.024(5) 0.017(6) N8 0.127(8) 0.138(9) 0.061(5) 0.009(5) 0.002(5) -0.045(7) N9 0.168(12) 0.198(15) 0.115(10) 0.019(10) -0.027(9) -0.068(12) _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 Co C5 2.063(7) . ? Co C2 2.069(7) . ? Co C3 2.070(8) . ? Co C4 2.083(8) . ? Co C1 2.086(7) . ? Co P1 2.1467(18) . ? Co P2 2.1511(18) . ? Co P3 2.1537(19) . ? C1 C2 1.430(12) . ? C1 C5 1.438(12) . ? C2 C3 1.402(13) . ? C3 C4 1.390(15) . ? C4 C5 1.388(14) . ? P1 O3 1.513(5) . ? P1 O1 1.578(5) . ? P1 O2 1.585(6) . ? O1 C11 1.452(10) . ? C11 C12 1.366(19) . ? O2 C21A 1.359(14) . ? O2 C21 1.40(2) . ? C21 C22 1.30(4) . ? C21A C22 1.37(2) . ? O3 Ge 1.885(6) . ? P2 O6 1.549(5) . ? P2 O4 1.573(6) . ? P2 O5 1.584(6) . ? O4 C41 1.448(10) . ? C41 C42 1.459(13) . ? O5 C51 1.367(13) . ? C51 C52 1.516(12) . ? O6 Ge 1.884(5) . ? P3 O7 1.550(6) . ? P3 O9 1.558(6) . ? P3 O8 1.579(6) . ? O7 C71 1.530(12) . ? C71 C72 1.366(17) . ? O8 C81 1.398(14) . ? C81 C82 1.30(2) . ? O9 Ge 1.909(6) . ? Ge N4 1.926(7) . ? Ge N1 1.935(8) . ? Ge N7 1.960(9) . ? N1 N2 1.166(10) . ? N2 N3 1.091(12) . ? N4 N5 1.163(11) . ? N5 N6 1.149(12) . ? N7 N8 1.163(14) . ? N8 N9 1.116(16) . ? 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 C5 Co C2 67.1(3) . . ? C5 Co C3 65.9(4) . . ? C2 Co C3 39.6(4) . . ? C5 Co C4 39.1(4) . . ? C2 Co C4 66.5(4) . . ? C3 Co C4 39.1(4) . . ? C5 Co C1 40.5(3) . . ? C2 Co C1 40.2(3) . . ? C3 Co C1 66.9(3) . . ? C4 Co C1 67.0(3) . . ? C5 Co P1 89.9(3) . . ? C2 Co P1 140.7(3) . . ? C3 Co P1 153.8(3) . . ? C4 Co P1 115.1(3) . . ? C1 Co P1 101.9(2) . . ? C5 Co P2 142.4(3) . . ? C2 Co P2 90.7(2) . . ? C3 Co P2 115.7(3) . . ? C4 Co P2 154.6(3) . . ? C1 Co P2 103.2(2) . . ? P1 Co P2 89.51(7) . . ? C5 Co P3 125.9(3) . . ? C2 Co P3 130.0(3) . . ? C3 Co P3 96.7(3) . . ? C4 Co P3 94.8(3) . . ? C1 Co P3 161.3(2) . . ? P1 Co P3 89.23(7) . . ? P2 Co P3 91.68(7) . . ? C2 C1 C5 105.6(8) . . ? C2 C1 Co 69.2(4) . . ? C5 C1 Co 68.9(4) . . ? C3 C2 C1 107.9(8) . . ? C3 C2 Co 70.2(4) . . ? C1 C2 Co 70.5(4) . . ? C4 C3 C2 109.3(8) . . ? C4 C3 Co 70.9(5) . . ? C2 C3 Co 70.2(4) . . ? C5 C4 C3 108.1(8) . . ? C5 C4 Co 69.7(4) . . ? C3 C4 Co 70.0(5) . . ? C4 C5 C1 109.0(8) . . ? C4 C5 Co 71.2(5) . . ? C1 C5 Co 70.6(4) . . ? O3 P1 O1 108.3(4) . . ? O3 P1 O2 106.1(4) . . ? O1 P1 O2 99.6(4) . . ? O3 P1 Co 116.8(2) . . ? O1 P1 Co 109.73(19) . . ? O2 P1 Co 114.8(2) . . ? C11 O1 P1 121.3(6) . . ? C12 C11 O1 114.9(11) . . ? C21A O2 C21 47.0(15) . . ? C21A O2 P1 133.6(8) . . ? C21 O2 P1 117.3(15) . . ? C22 C21 O2 118(3) . . ? O2 C21A C22 116.5(17) . . ? C21 C22 C21A 48.6(13) . . ? P1 O3 Ge 133.7(3) . . ? O6 P2 O4 107.8(3) . . ? O6 P2 O5 107.3(3) . . ? O4 P2 O5 100.0(4) . . ? O6 P2 Co 116.7(2) . . ? O4 P2 Co 109.0(2) . . ? O5 P2 Co 114.6(3) . . ? C41 O4 P2 122.6(5) . . ? O4 C41 C42 110.6(8) . . ? C51 O5 P2 128.6(6) . . ? O5 C51 C52 109.4(8) . . ? P2 O6 Ge 131.3(3) . . ? O7 P3 O9 109.0(4) . . ? O7 P3 O8 102.8(4) . . ? O9 P3 O8 105.6(3) . . ? O7 P3 Co 110.1(2) . . ? O9 P3 Co 116.2(2) . . ? O8 P3 Co 112.2(2) . . ? C71 O7 P3 118.6(6) . . ? C72 C71 O7 111.3(10) . . ? C81 O8 P3 129.3(10) . . ? C82 C81 O8 119.7(16) . . ? P3 O9 Ge 132.5(3) . . ? O6 Ge O3 91.4(3) . . ? O6 Ge O9 88.5(3) . . ? O3 Ge O9 89.7(3) . . ? O6 Ge N4 90.1(3) . . ? O3 Ge N4 178.2(3) . . ? O9 Ge N4 91.3(3) . . ? O6 Ge N1 92.1(3) . . ? O3 Ge N1 86.5(3) . . ? O9 Ge N1 176.2(3) . . ? N4 Ge N1 92.4(3) . . ? O6 Ge N7 175.4(3) . . ? O3 Ge N7 84.2(4) . . ? O9 Ge N7 90.1(4) . . ? N4 Ge N7 94.3(4) . . ? N1 Ge N7 89.0(4) . . ? N2 N1 Ge 121.5(6) . . ? N3 N2 N1 174.1(9) . . ? N5 N4 Ge 121.1(6) . . ? N6 N5 N4 176.6(8) . . ? N8 N7 Ge 118.6(9) . . ? N9 N8 N7 171.9(14) . . ? _diffrn_measured_fraction_theta_max 0.501 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.501 _refine_diff_density_max 1.366 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.096