# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_Zn(en)3[Ga2Ge4O12] _database_code_depnum_ccdc_archive 'CCDC 884752' #TrackingRef '11628_web_deposit_cif_file_0_xuyan_1338453798.Zn(en)3[Ga2Ge4O12].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Zn(en)3[Ga2Ge4O12] _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H8 Ga0.67 Ge1.33 N2 O4 Zn0.33' _chemical_formula_weight 289.16 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 '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 Cubic _symmetry_space_group_name_H-M 'P a -3' 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' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' _cell_length_a 16.563(2) _cell_length_b 16.563(2) _cell_length_c 16.563(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4543.9(10) _cell_formula_units_Z 24 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3344 _exptl_absorpt_coefficient_mu 8.657 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3946 _exptl_absorpt_correction_T_max 0.6652 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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_reflns_number 29458 _diffrn_reflns_av_R_equivalents 0.1639 _diffrn_reflns_av_sigmaI/netI 0.0574 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 28.32 _reflns_number_total 1899 _reflns_number_gt 1419 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0804P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1899 _refine_ls_number_parameters 94 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1291 _refine_ls_wR_factor_gt 0.1250 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.033 _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 Ga1 Ga 0.84107(4) 0.06556(4) 0.07756(4) 0.0171(2) Uani 0.33 1 d P . . Ge1 Ge 0.84107(4) 0.06556(4) 0.07756(4) 0.0171(2) Uani 0.67 1 d P . . Ga2 Ga 0.86073(4) 0.25582(4) 0.08981(4) 0.0158(2) Uani 0.33 1 d P . . Ge2 Ge 0.86073(4) 0.25582(4) 0.08981(4) 0.0158(2) Uani 0.67 1 d P . . Zn1 Zn 1.16720(5) 0.16720(5) 0.16720(5) 0.0289(3) Uani 1 3 d S . . O1 O 0.7565(3) 0.0008(3) 0.0848(3) 0.0327(12) Uani 1 1 d . . . O2 O 0.8672(3) 0.0775(3) -0.0247(3) 0.0283(10) Uani 1 1 d . . . O3 O 0.8167(3) 0.1618(3) 0.1173(3) 0.0287(11) Uani 1 1 d . . . O4 O 0.7866(3) 0.3301(3) 0.0750(3) 0.0304(11) Uani 1 1 d . . . N1 N 1.3003(5) 0.1599(5) 0.1702(7) 0.085(3) Uani 1 1 d U . . H1A H 1.3216 0.1926 0.1324 0.102 Uiso 1 1 calc R . . H1B H 1.3188 0.1754 0.2188 0.102 Uiso 1 1 calc R . . N2 N 1.1858(4) 0.0394(4) 0.1509(4) 0.0470(17) Uani 1 1 d U . . H2A H 1.1698 0.0132 0.1957 0.056 Uiso 1 1 calc R . . H2B H 1.1553 0.0221 0.1095 0.056 Uiso 1 1 calc R . . C1 C 1.3210(7) 0.0840(7) 0.1558(10) 0.105(3) Uani 1 1 d DU . . H1C H 1.3496 0.0660 0.2036 0.125 Uiso 1 1 calc R . . H1D H 1.3608 0.0862 0.1128 0.125 Uiso 1 1 calc R . . C2 C 1.2683(6) 0.0205(6) 0.1351(8) 0.080(3) Uani 1 1 d DU . . H2C H 1.2831 -0.0273 0.1655 0.096 Uiso 1 1 calc R . . H2D H 1.2745 0.0082 0.0782 0.096 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 Ga1 0.0182(3) 0.0133(3) 0.0197(3) 0.0022(2) 0.0009(2) -0.0014(2) Ge1 0.0182(3) 0.0133(3) 0.0197(3) 0.0022(2) 0.0009(2) -0.0014(2) Ga2 0.0190(3) 0.0143(3) 0.0141(3) -0.0027(2) 0.0000(2) 0.0029(2) Ge2 0.0190(3) 0.0143(3) 0.0141(3) -0.0027(2) 0.0000(2) 0.0029(2) Zn1 0.0289(3) 0.0289(3) 0.0289(3) -0.0020(3) -0.0020(3) -0.0020(3) O1 0.022(2) 0.028(2) 0.048(3) 0.018(2) -0.009(2) -0.006(2) O2 0.043(3) 0.021(2) 0.021(2) -0.0034(18) 0.004(2) -0.009(2) O3 0.037(3) 0.024(2) 0.026(2) 0.0005(19) 0.014(2) -0.003(2) O4 0.032(3) 0.032(3) 0.028(2) -0.010(2) -0.017(2) 0.016(2) N1 0.042(4) 0.054(5) 0.159(8) -0.006(5) -0.022(5) -0.017(4) N2 0.055(4) 0.032(3) 0.055(4) -0.002(3) -0.002(3) -0.011(3) C1 0.056(5) 0.085(6) 0.173(8) -0.034(6) -0.020(6) 0.011(5) C2 0.061(5) 0.058(5) 0.122(7) -0.013(5) 0.000(5) 0.013(5) _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 Ga1 O2 1.759(4) . ? Ga1 O2 1.766(4) 21_656 ? Ga1 O1 1.768(4) . ? Ga1 O3 1.771(4) . ? Ga2 O4 1.755(4) . ? Ga2 O1 1.764(4) 17_665 ? Ga2 O4 1.776(4) 8_645 ? Ga2 O3 1.778(4) . ? Zn1 N2 2.155(6) . ? Zn1 N2 2.155(6) 5_645 ? Zn1 N2 2.155(6) 9_654 ? Zn1 N1 2.208(8) 5_645 ? Zn1 N1 2.208(8) 9_654 ? Zn1 N1 2.208(8) . ? O1 Ge2 1.764(4) 21_656 ? O1 Ga2 1.764(4) 21_656 ? O2 Ge1 1.766(4) 17_665 ? O2 Ga1 1.766(4) 17_665 ? O4 Ge2 1.776(4) 11_556 ? O4 Ga2 1.776(4) 11_556 ? N1 C1 1.325(13) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C2 1.426(11) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? C1 C2 1.409(9) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? 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 O2 Ga1 O2 110.8(3) . 21_656 ? O2 Ga1 O1 109.1(2) . . ? O2 Ga1 O1 109.7(2) 21_656 . ? O2 Ga1 O3 108.2(2) . . ? O2 Ga1 O3 109.0(2) 21_656 . ? O1 Ga1 O3 109.9(2) . . ? O4 Ga2 O1 108.6(2) . 17_665 ? O4 Ga2 O4 108.8(3) . 8_645 ? O1 Ga2 O4 111.2(2) 17_665 8_645 ? O4 Ga2 O3 111.3(2) . . ? O1 Ga2 O3 109.1(2) 17_665 . ? O4 Ga2 O3 107.8(2) 8_645 . ? N2 Zn1 N2 92.1(3) . 5_645 ? N2 Zn1 N2 92.1(3) . 9_654 ? N2 Zn1 N2 92.1(3) 5_645 9_654 ? N2 Zn1 N1 165.9(3) . 5_645 ? N2 Zn1 N1 78.8(3) 5_645 5_645 ? N2 Zn1 N1 98.9(4) 9_654 5_645 ? N2 Zn1 N1 98.9(4) . 9_654 ? N2 Zn1 N1 165.9(3) 5_645 9_654 ? N2 Zn1 N1 78.8(3) 9_654 9_654 ? N1 Zn1 N1 91.9(4) 5_645 9_654 ? N2 Zn1 N1 78.8(3) . . ? N2 Zn1 N1 98.9(4) 5_645 . ? N2 Zn1 N1 165.9(3) 9_654 . ? N1 Zn1 N1 91.9(4) 5_645 . ? N1 Zn1 N1 91.9(4) 9_654 . ? Ge2 O1 Ga2 0.00(5) 21_656 21_656 ? Ge2 O1 Ga1 130.0(2) 21_656 . ? Ga2 O1 Ga1 130.0(2) 21_656 . ? Ga1 O2 Ge1 125.6(2) . 17_665 ? Ga1 O2 Ga1 125.6(2) . 17_665 ? Ge1 O2 Ga1 0.00(6) 17_665 17_665 ? Ga1 O3 Ga2 126.8(3) . . ? Ga2 O4 Ge2 129.8(3) . 11_556 ? Ga2 O4 Ga2 129.8(3) . 11_556 ? Ge2 O4 Ga2 0.00(6) 11_556 11_556 ? C1 N1 Zn1 107.9(7) . . ? C1 N1 H1A 110.1 . . ? Zn1 N1 H1A 110.1 . . ? C1 N1 H1B 110.1 . . ? Zn1 N1 H1B 110.1 . . ? H1A N1 H1B 108.4 . . ? C2 N2 Zn1 112.1(5) . . ? C2 N2 H2A 109.2 . . ? Zn1 N2 H2A 109.2 . . ? C2 N2 H2B 109.2 . . ? Zn1 N2 H2B 109.2 . . ? H2A N2 H2B 107.9 . . ? N1 C1 C2 126.3(11) . . ? N1 C1 H1C 105.8 . . ? C2 C1 H1C 105.8 . . ? N1 C1 H1D 105.8 . . ? C2 C1 H1D 105.8 . . ? H1C C1 H1D 106.2 . . ? C1 C2 N2 112.6(9) . . ? C1 C2 H2C 109.1 . . ? N2 C2 H2C 109.1 . . ? C1 C2 H2D 109.1 . . ? N2 C2 H2D 109.1 . . ? H2C C2 H2D 107.8 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.220 _refine_diff_density_min -1.664 _refine_diff_density_rms 0.284 data_Co(en)3[Ga2Ge4O12] _database_code_depnum_ccdc_archive 'CCDC 884753' #TrackingRef '11629_web_deposit_cif_file_1_xuyan_1338453798.Co(en)3[Ga2Ge4O12].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Co(en)3[Ga2Ge4O12] _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H8 Co0.33 Ga0.67 Ge1.33 N2 O4' _chemical_formula_weight 287.01 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' Ga Ga 0.2307 1.6083 '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 Cubic _symmetry_space_group_name_H-M 'P a -3' 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' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' _cell_length_a 16.5903(5) _cell_length_b 16.5903(5) _cell_length_c 16.5903(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4566.3(2) _cell_formula_units_Z 24 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3320 _exptl_absorpt_coefficient_mu 8.291 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4861 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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_reflns_number 32047 _diffrn_reflns_av_R_equivalents 0.0608 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 28.34 _reflns_number_total 1914 _reflns_number_gt 1640 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1914 _refine_ls_number_parameters 94 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.1227 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 1.032 _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 Ga1 Ga 0.84097(3) 0.06633(3) 0.07716(3) 0.01789(18) Uani 0.33 1 d P . . Ge1 Ge 0.84097(3) 0.06633(3) 0.07716(3) 0.01789(18) Uani 0.67 1 d P . . Ga2 Ga 0.86137(3) 0.25662(2) 0.08878(2) 0.01680(17) Uani 0.33 1 d P . . Ge2 Ge 0.86137(3) 0.25662(2) 0.08878(2) 0.01680(17) Uani 0.67 1 d P . . Co1 Co 0.16710(4) 0.16710(4) 0.16710(4) 0.0247(3) Uani 1 3 d S . . O1 O 0.75603(19) 0.0021(2) 0.0848(2) 0.0332(9) Uani 1 1 d . . . O2 O 0.8674(2) 0.07792(18) -0.02548(19) 0.0293(7) Uani 1 1 d . . . O3 O 0.8174(2) 0.16334(18) 0.1167(2) 0.0294(7) Uani 1 1 d . . . O4 O 0.9262(2) 0.2872(2) 0.16831(19) 0.0316(8) Uani 1 1 d . . . C1 C 0.0208(4) 0.1374(7) 0.2684(4) 0.087(3) Uani 1 1 d DU . . H1A H -0.0271 0.1678 0.2827 0.104 Uiso 1 1 calc R . . H1B H 0.0087 0.0806 0.2756 0.104 Uiso 1 1 calc R . . C2 C 0.0825(5) 0.1586(7) 0.3196(5) 0.100(3) Uani 1 1 d DU . . H2A H 0.0669 0.2098 0.3431 0.120 Uiso 1 1 calc R . . H2B H 0.0814 0.1196 0.3631 0.120 Uiso 1 1 calc R . . N1 N 0.1846(3) 0.0399(3) 0.1520(3) 0.0394(11) Uani 1 1 d . . . H1C H 0.1678 0.0140 0.1966 0.047 Uiso 1 1 calc R . . H1D H 0.1547 0.0225 0.1102 0.047 Uiso 1 1 calc R . . N2 N 0.1588(3) 0.1663(5) 0.2995(3) 0.081(2) Uani 1 1 d U . . H2C H 0.1876 0.1250 0.3196 0.097 Uiso 1 1 calc R . . H2D H 0.1787 0.2126 0.3196 0.097 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 Ga1 0.0186(3) 0.0146(2) 0.0205(2) 0.00236(16) 0.00086(16) -0.00181(15) Ge1 0.0186(3) 0.0146(2) 0.0205(2) 0.00236(16) 0.00086(16) -0.00181(15) Ga2 0.0194(3) 0.0155(2) 0.0155(2) -0.00301(15) -0.00003(15) 0.00296(16) Ge2 0.0194(3) 0.0155(2) 0.0155(2) -0.00301(15) -0.00003(15) 0.00296(16) Co1 0.0247(3) 0.0247(3) 0.0247(3) -0.0024(2) -0.0024(2) -0.0024(2) O1 0.0240(16) 0.0305(19) 0.045(2) 0.0177(15) -0.0088(14) -0.0107(14) O2 0.045(2) 0.0233(16) 0.0200(15) -0.0020(12) 0.0013(14) -0.0069(14) O3 0.0380(18) 0.0223(16) 0.0279(17) -0.0002(12) 0.0148(14) -0.0005(13) O4 0.0316(18) 0.0319(18) 0.0313(18) -0.0143(14) -0.0099(14) 0.0159(14) C1 0.046(4) 0.158(8) 0.058(4) 0.023(5) 0.021(3) -0.006(5) C2 0.077(5) 0.184(7) 0.039(3) -0.014(4) 0.018(3) -0.045(5) N1 0.051(3) 0.028(2) 0.039(2) 0.0037(18) -0.001(2) -0.008(2) N2 0.052(3) 0.159(7) 0.031(3) -0.016(3) -0.010(2) 0.003(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 Ga1 O2 1.765(3) 21_656 ? Ga1 O2 1.769(3) . ? Ga1 O1 1.771(3) . ? Ga1 O3 1.781(3) . ? Ga2 O1 1.765(3) 17_665 ? Ga2 O4 1.768(3) 11_556 ? Ga2 O3 1.772(3) . ? Ga2 O4 1.776(3) . ? Co1 N1 2.145(4) 5 ? Co1 N1 2.145(4) 9 ? Co1 N1 2.145(4) . ? Co1 N2 2.200(5) . ? Co1 N2 2.200(5) 9 ? Co1 N2 2.200(5) 5 ? O1 Ge2 1.765(3) 21_656 ? O1 Ga2 1.765(3) 21_656 ? O2 Ge1 1.765(3) 17_665 ? O2 Ga1 1.765(3) 17_665 ? O4 Ge2 1.768(3) 8_645 ? O4 Ga2 1.768(3) 8_645 ? C1 C2 1.376(8) . ? C1 N1 1.447(8) 9 ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.315(9) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? N1 C1 1.447(8) 5 ? N1 H1C 0.9000 . ? N1 H1D 0.9000 . ? N2 H2C 0.9000 . ? N2 H2D 0.9000 . ? 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 O2 Ga1 O2 110.8(2) 21_656 . ? O2 Ga1 O1 109.78(15) 21_656 . ? O2 Ga1 O1 109.33(16) . . ? O2 Ga1 O3 108.79(16) 21_656 . ? O2 Ga1 O3 108.10(14) . . ? O1 Ga1 O3 110.05(16) . . ? O1 Ga2 O4 108.42(17) 17_665 11_556 ? O1 Ga2 O3 109.13(14) 17_665 . ? O4 Ga2 O3 111.45(16) 11_556 . ? O1 Ga2 O4 111.23(16) 17_665 . ? O4 Ga2 O4 108.91(18) 11_556 . ? O3 Ga2 O4 107.73(18) . . ? N1 Co1 N1 91.95(18) 5 9 ? N1 Co1 N1 91.95(18) 5 . ? N1 Co1 N1 91.95(18) 9 . ? N1 Co1 N2 167.3(2) 5 . ? N1 Co1 N2 78.6(2) 9 . ? N1 Co1 N2 96.8(3) . . ? N1 Co1 N2 78.6(2) 5 9 ? N1 Co1 N2 96.8(3) 9 9 ? N1 Co1 N2 167.3(2) . 9 ? N2 Co1 N2 93.9(3) . 9 ? N1 Co1 N2 96.8(3) 5 5 ? N1 Co1 N2 167.3(2) 9 5 ? N1 Co1 N2 78.6(2) . 5 ? N2 Co1 N2 93.9(3) . 5 ? N2 Co1 N2 93.9(3) 9 5 ? Ge2 O1 Ga2 0.00(4) 21_656 21_656 ? Ge2 O1 Ga1 130.13(18) 21_656 . ? Ga2 O1 Ga1 130.13(18) 21_656 . ? Ge1 O2 Ga1 0.00(4) 17_665 17_665 ? Ge1 O2 Ga1 125.55(17) 17_665 . ? Ga1 O2 Ga1 125.55(17) 17_665 . ? Ga2 O3 Ga1 127.04(18) . . ? Ge2 O4 Ga2 0.00(4) 8_645 8_645 ? Ge2 O4 Ga2 129.58(18) 8_645 . ? Ga2 O4 Ga2 129.58(18) 8_645 . ? C2 C1 N1 112.7(6) . 9 ? C2 C1 H1A 109.0 . . ? N1 C1 H1A 109.0 9 . ? C2 C1 H1B 109.0 . . ? N1 C1 H1B 109.0 9 . ? H1A C1 H1B 107.8 . . ? N2 C2 C1 125.8(7) . . ? N2 C2 H2A 105.9 . . ? C1 C2 H2A 105.9 . . ? N2 C2 H2B 105.9 . . ? C1 C2 H2B 105.9 . . ? H2A C2 H2B 106.2 . . ? C1 N1 Co1 111.4(4) 5 . ? C1 N1 H1C 109.3 5 . ? Co1 N1 H1C 109.3 . . ? C1 N1 H1D 109.3 5 . ? Co1 N1 H1D 109.3 . . ? H1C N1 H1D 108.0 . . ? C2 N2 Co1 108.3(5) . . ? C2 N2 H2C 110.0 . . ? Co1 N2 H2C 110.0 . . ? C2 N2 H2D 110.0 . . ? Co1 N2 H2D 110.0 . . ? H2C N2 H2D 108.4 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.836 _refine_diff_density_min -1.289 _refine_diff_density_rms 0.136 data_Co(en)3[Al2Ge4O12] _database_code_depnum_ccdc_archive 'CCDC 884754' #TrackingRef '11630_web_deposit_cif_file_2_xuyan_1338453798.Co(en)3[Al2Ge4O12].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Co(en)3[Al2Ge4O12] _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H24 Al2 Co Ge4 N6 O12' _chemical_formula_weight 775.56 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' Al Al 0.0645 0.0514 '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' Ge Ge 0.1547 1.8001 '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' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Pa-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' 'z, x, y' '-z+1/2, -x, y+1/2' 'z+1/2, -x+1/2, -y' '-z, x+1/2, -y+1/2' 'y, z, x' 'y+1/2, -z+1/2, -x' '-y, z+1/2, -x+1/2' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' '-z, -x, -y' 'z-1/2, x, -y-1/2' '-z-1/2, x-1/2, y' 'z, -x-1/2, y-1/2' '-y, -z, -x' '-y-1/2, z-1/2, x' 'y, -z-1/2, x-1/2' 'y-1/2, z, -x-1/2' _cell_length_a 16.4770(2) _cell_length_b 16.4770(2) _cell_length_c 16.4770(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4473.37(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9603 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 28.23 _exptl_crystal_description BLOCK _exptl_crystal_colour BROWN _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3032 _exptl_absorpt_coefficient_mu 6.184 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.2763 _exptl_absorpt_correction_T_max 0.3070 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 5.0cm _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31153 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.0157 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 28.23 _reflns_number_total 1843 _reflns_number_gt 1693 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0360P)^2^+25.2175P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1843 _refine_ls_number_parameters 94 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0859 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.045 _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 0.43587(3) 0.92139(3) 0.34148(3) 0.01385(13) Uani 0.67 1 d P . . Al1 Al 0.43587(3) 0.92139(3) 0.34148(3) 0.01385(13) Uani 0.33 1 d P . . Ge2 Ge 0.24559(3) 0.90834(3) 0.35992(3) 0.01346(13) Uani 0.67 1 d P . . Al2 Al 0.24559(3) 0.90834(3) 0.35992(3) 0.01346(13) Uani 0.33 1 d P . . Co1 Co 0.16721(3) 0.16721(3) 0.16721(3) 0.0238(2) Uani 1 3 d S . . O1 O 0.34001(15) 0.88135(17) 0.31843(17) 0.0224(6) Uani 1 1 d . . . O2 O 0.47720(16) 0.86696(19) 0.42268(16) 0.0238(6) Uani 1 1 d . . . O3 O 0.50126(17) 0.91349(18) 0.25839(16) 0.0244(6) Uani 1 1 d . . . O4 O 0.17155(17) 0.92258(17) 0.28552(17) 0.0229(6) Uani 1 1 d . . . N1 N 0.1511(3) 0.1849(3) 0.0393(2) 0.0378(9) Uani 1 1 d . . . H1N1 H 0.1955 0.1671 0.0128 0.045 Uiso 1 1 calc R . . H2N1 H 0.1083 0.1556 0.0222 0.045 Uiso 1 1 calc R . . N2 N 0.1648(5) 0.2996(3) 0.1600(3) 0.0685(17) Uani 1 1 d U . . H1N2 H 0.1258 0.3194 0.1928 0.082 Uiso 1 1 calc R . . H2N2 H 0.2128 0.3201 0.1761 0.082 Uiso 1 1 calc R . . C1 C 0.1378(6) 0.2702(4) 0.0204(4) 0.079(2) Uani 1 1 d U . . H1C1 H 0.1737 0.2853 -0.0237 0.094 Uiso 1 1 calc R . . H2C1 H 0.0826 0.2766 0.0012 0.094 Uiso 1 1 calc R . . C2 C 0.1497(8) 0.3215(5) 0.0814(6) 0.123(4) Uani 1 1 d U . . H1C2 H 0.1020 0.3560 0.0831 0.148 Uiso 1 1 calc R . . H2C2 H 0.1945 0.3560 0.0652 0.148 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 0.0110(2) 0.0159(2) 0.0146(2) -0.00063(16) 0.00134(16) 0.00154(16) Al1 0.0110(2) 0.0159(2) 0.0146(2) -0.00063(16) 0.00134(16) 0.00154(16) Ge2 0.0124(2) 0.0127(2) 0.0152(2) -0.00013(16) -0.00201(16) -0.00223(16) Al2 0.0124(2) 0.0127(2) 0.0152(2) -0.00013(16) -0.00201(16) -0.00223(16) Co1 0.0238(2) 0.0238(2) 0.0238(2) -0.0023(2) -0.0023(2) -0.0023(2) O1 0.0131(12) 0.0254(14) 0.0288(14) -0.0109(11) -0.0009(10) -0.0004(10) O2 0.0167(12) 0.0366(16) 0.0183(13) 0.0079(11) 0.0016(10) 0.0042(11) O3 0.0209(13) 0.0342(15) 0.0180(13) 0.0057(11) 0.0051(10) 0.0124(12) O4 0.0208(13) 0.0234(13) 0.0245(14) 0.0089(11) -0.0104(11) -0.0071(11) N1 0.040(2) 0.049(2) 0.0247(18) -0.0086(17) 0.0026(16) 0.0014(19) N2 0.129(5) 0.033(2) 0.044(3) -0.013(2) -0.001(3) -0.005(3) C1 0.139(7) 0.060(4) 0.037(3) 0.012(3) 0.000(4) 0.032(4) C2 0.238(10) 0.032(3) 0.100(6) 0.016(4) -0.081(7) -0.016(5) _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 O2 1.736(3) 20_575 ? Ge1 O3 1.747(3) . ? Ge1 O2 1.749(3) . ? Ge1 O1 1.753(3) . ? Ge2 O3 1.744(3) 20_575 ? Ge2 O4 1.745(3) . ? Ge2 O4 1.750(3) 6_564 ? Ge2 O1 1.756(3) . ? Co1 N1 2.144(4) 5 ? Co1 N1 2.144(4) . ? Co1 N1 2.144(4) 9 ? Co1 N2 2.186(5) 5 ? Co1 N2 2.186(5) 9 ? Co1 N2 2.186(5) . ? O2 Al1 1.736(3) 22_765 ? O2 Ge1 1.736(3) 22_765 ? O3 Al2 1.744(3) 22_765 ? O3 Ge2 1.744(3) 22_765 ? O4 Al2 1.750(3) 11_655 ? O4 Ge2 1.750(3) 11_655 ? N1 C1 1.457(8) . ? N1 H1N1 0.9000 . ? N1 H2N1 0.9000 . ? N2 C2 1.367(10) . ? N2 H1N2 0.9000 . ? N2 H2N2 0.9000 . ? C1 C2 1.328(11) . ? C1 H1C1 0.9700 . ? C1 H2C1 0.9700 . ? C2 H1C2 0.9700 . ? C2 H2C2 0.9700 . ? 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 O2 Ge1 O3 109.78(14) 20_575 . ? O2 Ge1 O2 110.9(2) 20_575 . ? O3 Ge1 O2 108.73(13) . . ? O2 Ge1 O1 107.57(13) 20_575 . ? O3 Ge1 O1 110.96(14) . . ? O2 Ge1 O1 108.88(14) . . ? O3 Ge2 O4 108.97(14) 20_575 . ? O3 Ge2 O4 112.29(14) 20_575 6_564 ? O4 Ge2 O4 108.11(16) . 6_564 ? O3 Ge2 O1 107.82(12) 20_575 . ? O4 Ge2 O1 112.32(14) . . ? O4 Ge2 O1 107.38(14) 6_564 . ? N1 Co1 N1 91.64(17) 5 . ? N1 Co1 N1 91.64(17) 5 9 ? N1 Co1 N1 91.64(17) . 9 ? N1 Co1 N2 78.99(18) 5 5 ? N1 Co1 N2 167.7(2) . 5 ? N1 Co1 N2 96.5(2) 9 5 ? N1 Co1 N2 167.7(2) 5 9 ? N1 Co1 N2 96.5(2) . 9 ? N1 Co1 N2 78.99(18) 9 9 ? N2 Co1 N2 94.1(2) 5 9 ? N1 Co1 N2 96.5(2) 5 . ? N1 Co1 N2 78.99(18) . . ? N1 Co1 N2 167.7(2) 9 . ? N2 Co1 N2 94.1(2) 5 . ? N2 Co1 N2 94.1(2) 9 . ? Ge1 O1 Ge2 128.19(16) . . ? Al1 O2 Ge1 0.00(4) 22_765 22_765 ? Al1 O2 Ge1 126.47(16) 22_765 . ? Ge1 O2 Ge1 126.47(16) 22_765 . ? Al2 O3 Ge2 0.00(4) 22_765 22_765 ? Al2 O3 Ge1 131.23(16) 22_765 . ? Ge2 O3 Ge1 131.23(16) 22_765 . ? Ge2 O4 Al2 130.71(16) . 11_655 ? Ge2 O4 Ge2 130.71(16) . 11_655 ? Al2 O4 Ge2 0.000(19) 11_655 11_655 ? C1 N1 Co1 111.1(3) . . ? C1 N1 H1N1 109.4 . . ? Co1 N1 H1N1 109.4 . . ? C1 N1 H2N1 109.4 . . ? Co1 N1 H2N1 109.4 . . ? H1N1 N1 H2N1 108.0 . . ? C2 N2 Co1 108.5(4) . . ? C2 N2 H1N2 110.0 . . ? Co1 N2 H1N2 110.0 . . ? C2 N2 H2N2 110.0 . . ? Co1 N2 H2N2 110.0 . . ? H1N2 N2 H2N2 108.4 . . ? C2 C1 N1 115.5(6) . . ? C2 C1 H1C1 108.4 . . ? N1 C1 H1C1 108.4 . . ? C2 C1 H2C1 108.4 . . ? N1 C1 H2C1 108.4 . . ? H1C1 C1 H2C1 107.5 . . ? C1 C2 N2 125.2(7) . . ? C1 C2 H1C2 106.0 . . ? N2 C2 H1C2 106.0 . . ? C1 C2 H2C2 106.0 . . ? N2 C2 H2C2 106.0 . . ? H1C2 C2 H2C2 106.3 . . ? 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 N2 H1N2 O1 0.90 2.38 2.938(6) 120.6 15_655 N1 H2N1 O2 0.90 2.19 2.982(5) 146.0 2_564 N1 H1N1 O4 0.90 2.10 2.941(5) 154.8 5_554 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.23 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.855 _refine_diff_density_min -1.089 _refine_diff_density_rms 0.114 data_Ni(en)3[Al2Ge4O12] _database_code_depnum_ccdc_archive 'CCDC 884755' #TrackingRef '11631_web_deposit_cif_file_3_xuyan_1338453798.Ni(en)3[Al2Ge4O12].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Ni(en)3[Al2Ge4O12] _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H8 Al0.67 Ge1.33 N2 Ni0.33 O4' _chemical_formula_weight 258.45 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' 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M 'P a -3' 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' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' _cell_length_a 16.4433(2) _cell_length_b 16.4433(2) _cell_length_c 16.4433(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4445.97(9) _cell_formula_units_Z 24 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3040 _exptl_absorpt_coefficient_mu 6.323 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6395 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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_reflns_number 31222 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0165 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 28.29 _reflns_number_total 1843 _reflns_number_gt 1602 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+10.2559P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1843 _refine_ls_number_parameters 94 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0919 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.073 _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 0.84115(3) 0.06636(3) 0.07738(3) 0.01506(14) Uani 0.67 1 d P . . Al1 Al 0.84115(3) 0.06636(3) 0.07738(3) 0.01506(14) Uani 0.33 1 d P . . Ge2 Ge 0.86161(3) 0.25677(3) 0.08880(3) 0.01476(14) Uani 0.67 1 d P . . Al2 Al 0.86161(3) 0.25677(3) 0.08880(3) 0.01476(14) Uani 0.33 1 d P . . O1 O 0.81932(16) 0.16294(14) 0.11685(17) 0.0246(5) Uani 1 1 d . . . O2 O 0.92530(16) 0.28803(16) 0.16802(15) 0.0247(6) Uani 1 1 d . . . O3 O 0.92156(15) 0.02420(15) 0.13258(17) 0.0248(5) Uani 1 1 d . . . O4 O 0.75685(15) 0.00215(15) 0.08553(16) 0.0256(6) Uani 1 1 d . . . Ni1 Ni 0.16643(3) 0.16643(3) 0.16643(3) 0.02163(19) Uani 1 3 d S . . N1 N 0.1823(2) 0.0405(2) 0.1525(2) 0.0347(8) Uani 1 1 d . . . H1A H 0.1645 0.0149 0.1974 0.042 Uiso 1 1 calc R . . H1B H 0.1526 0.0230 0.1100 0.042 Uiso 1 1 calc R . . N2 N 0.1626(4) 0.2968(3) 0.1618(3) 0.0603(14) Uani 1 1 d U . . H2A H 0.1202 0.3154 0.1908 0.072 Uiso 1 1 calc R . . H2B H 0.2086 0.3177 0.1830 0.072 Uiso 1 1 calc R . . C1 C 0.1389(5) 0.2678(4) 0.0205(4) 0.079(2) Uani 1 1 d U . . H1C H 0.1727 0.2818 -0.0258 0.095 Uiso 1 1 calc R . . H1D H 0.0827 0.2746 0.0042 0.095 Uiso 1 1 calc R . . C2 C 0.1549(6) 0.3203(4) 0.0811(5) 0.097(2) Uani 1 1 d U . . H2C H 0.1124 0.3612 0.0796 0.116 Uiso 1 1 calc R . . H2D H 0.2051 0.3478 0.0668 0.116 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 0.0154(2) 0.0125(2) 0.0173(2) 0.00161(15) 0.00030(15) -0.00141(15) Al1 0.0154(2) 0.0125(2) 0.0173(2) 0.00161(15) 0.00030(15) -0.00141(15) Ge2 0.0164(2) 0.0139(2) 0.0140(2) -0.00261(15) 0.00010(15) 0.00224(15) Al2 0.0164(2) 0.0139(2) 0.0140(2) -0.00261(15) 0.00010(15) 0.00224(15) O1 0.0290(13) 0.0175(12) 0.0274(14) -0.0016(10) 0.0095(11) 0.0004(10) O2 0.0234(13) 0.0275(13) 0.0231(13) -0.0116(10) -0.0080(10) 0.0102(10) O3 0.0201(12) 0.0177(12) 0.0366(15) 0.0054(10) -0.0070(10) -0.0005(9) O4 0.0193(12) 0.0229(13) 0.0347(14) 0.0133(11) -0.0062(10) -0.0070(10) Ni1 0.02163(19) 0.02163(19) 0.02163(19) -0.00209(16) -0.00209(16) -0.00209(16) N1 0.041(2) 0.0248(17) 0.038(2) 0.0035(14) 0.0024(16) -0.0058(15) N2 0.107(4) 0.030(2) 0.044(3) -0.0120(18) 0.004(2) -0.007(2) C1 0.150(6) 0.051(3) 0.036(3) 0.013(3) 0.005(3) 0.030(4) C2 0.177(6) 0.033(3) 0.081(4) 0.016(3) -0.042(4) -0.011(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 Ge1 O3 1.737(3) 17_665 ? Ge1 O3 1.747(2) . ? Ge1 O4 1.748(2) . ? Ge1 O1 1.753(2) . ? Ge2 O4 1.744(2) 17_665 ? Ge2 O2 1.745(2) 11_556 ? Ge2 O2 1.749(2) . ? Ge2 O1 1.754(2) . ? O2 Al2 1.745(2) 8_645 ? O2 Ge2 1.745(2) 8_645 ? O3 Al1 1.737(3) 21_656 ? O3 Ge1 1.737(3) 21_656 ? O4 Al2 1.744(2) 21_656 ? O4 Ge2 1.744(2) 21_656 ? Ni1 N1 2.099(3) . ? Ni1 N1 2.099(3) 9 ? Ni1 N1 2.099(3) 5 ? Ni1 N2 2.146(4) . ? Ni1 N2 2.146(4) 9 ? Ni1 N2 2.146(4) 5 ? N1 C1 1.461(7) 9 ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C2 1.387(8) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? C1 C2 1.344(9) . ? C1 N1 1.461(7) 5 ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? 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 O3 Ge1 O3 110.91(19) 17_665 . ? O3 Ge1 O4 109.88(13) 17_665 . ? O3 Ge1 O4 108.70(12) . . ? O3 Ge1 O1 107.66(12) 17_665 . ? O3 Ge1 O1 108.80(13) . . ? O4 Ge1 O1 110.89(12) . . ? O4 Ge2 O2 108.82(13) 17_665 11_556 ? O4 Ge2 O2 112.21(13) 17_665 . ? O2 Ge2 O2 107.80(15) 11_556 . ? O4 Ge2 O1 108.06(12) 17_665 . ? O2 Ge2 O1 112.54(13) 11_556 . ? O2 Ge2 O1 107.46(14) . . ? Ge1 O1 Ge2 128.20(15) . . ? Al2 O2 Ge2 0.00(4) 8_645 8_645 ? Al2 O2 Ge2 130.69(15) 8_645 . ? Ge2 O2 Ge2 130.69(15) 8_645 . ? Al1 O3 Ge1 0.00(3) 21_656 21_656 ? Al1 O3 Ge1 126.68(15) 21_656 . ? Ge1 O3 Ge1 126.68(15) 21_656 . ? Al2 O4 Ge2 0.00(4) 21_656 21_656 ? Al2 O4 Ge1 131.16(15) 21_656 . ? Ge2 O4 Ge1 131.16(15) 21_656 . ? N1 Ni1 N1 91.64(15) . 9 ? N1 Ni1 N1 91.64(15) . 5 ? N1 Ni1 N1 91.65(15) 9 5 ? N1 Ni1 N2 170.01(17) . . ? N1 Ni1 N2 94.87(19) 9 . ? N1 Ni1 N2 80.63(16) 5 . ? N1 Ni1 N2 80.63(16) . 9 ? N1 Ni1 N2 170.01(17) 9 9 ? N1 Ni1 N2 94.87(19) 5 9 ? N2 Ni1 N2 93.6(2) . 9 ? N1 Ni1 N2 94.87(19) . 5 ? N1 Ni1 N2 80.63(16) 9 5 ? N1 Ni1 N2 170.01(17) 5 5 ? N2 Ni1 N2 93.6(2) . 5 ? N2 Ni1 N2 93.6(2) 9 5 ? C1 N1 Ni1 111.0(3) 9 . ? C1 N1 H1A 109.4 9 . ? Ni1 N1 H1A 109.4 . . ? C1 N1 H1B 109.4 9 . ? Ni1 N1 H1B 109.4 . . ? H1A N1 H1B 108.0 . . ? C2 N2 Ni1 108.4(4) . . ? C2 N2 H2A 110.0 . . ? Ni1 N2 H2A 110.0 . . ? C2 N2 H2B 110.0 . . ? Ni1 N2 H2B 110.0 . . ? H2A N2 H2B 108.4 . . ? C2 C1 N1 114.9(5) . 5 ? C2 C1 H1C 108.5 . . ? N1 C1 H1C 108.5 5 . ? C2 C1 H1D 108.5 . . ? N1 C1 H1D 108.5 5 . ? H1C C1 H1D 107.5 . . ? C1 C2 N2 123.2(6) . . ? C1 C2 H2C 106.5 . . ? N2 C2 H2C 106.5 . . ? C1 C2 H2D 106.5 . . ? N2 C2 H2D 106.5 . . ? H2C C2 H2D 106.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.914 _refine_diff_density_min -1.167 _refine_diff_density_rms 0.107