# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name _publ_author_address 'Gregor Trimmel' ; Institut fur Materialchemie Technische Universitat Wien Getreidemarkt 9 A-1060 Wien Austria ; 'Christian Lembacher' ; Institut fur Materialchemie Technische Universitat Wien Getreidemarkt 9 A-1060 Wien Austria ; 'Guido Kickelbick' ; Institut fur Materialchemie Technische Universitat Wien Getreidemarkt 9 A-1060 Wien Austria ; 'Ulrich Schubert' ; Institut fur Anorganische Chemie Technische Universitat Wien Getreidemarkt 9 A-1060 Wien Austria ; _publ_contact_author_name 'Prof U Schubert' _publ_contact_author_address ; Institute of Inorganic Chemistry Technical University Vienna Getreidemarkt 9/153 A-1060 Vienna AUSTRIA ; _publ_contact_author_phone '+43 1 58801 15320' _publ_contact_author_fax '+43 1 58801 15399' _publ_contact_author_email 'uschuber@mail.zserv.tuwien.ac.at' _publ_requested_journal 'New. J. Chem.' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Sol-Gel Processing of Alkoxysilyl-Substituted Nickel Complexes for the Preparation of Highly Dispersed Nickel in Silica ; #============================================================================== data_rudi1 _database_code_CSD 184381 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C16 H30 N2 Ni O4' _chemical_formula_weight 373.13 _chemical_melting_point ? _chemical_compound_source ? 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 8.5048(3) _cell_length_b 10.2119(4) _cell_length_c 11.5220(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.2410(10) _cell_angle_gamma 90.00 _cell_volume 999.92(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.239 _exptl_crystal_density_method ? _exptl_crystal_F_000 400 _exptl_absorpt_coefficient_mu 0.988 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Siemens SMART CCD Detector' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time 20 _diffrn_standards_decay_% ? _diffrn_reflns_number 3817 _diffrn_reflns_av_R_equivalents 0.0718 _diffrn_reflns_av_sigmaI/netI 0.0576 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 23.26 _reflns_number_total 2612 _reflns_number_observed 2484 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART Software' _computing_cell_refinement 'Siemens SAINT Software' _computing_data_reduction 'Siemens SAINT Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL Software' _computing_publication_material 'Siemens SHELXTL Software' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0983P)^2^+0.1291P] 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 SHELXL _refine_ls_extinction_coef 0.0362(50) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 2612 _refine_ls_number_parameters 209 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_obs 0.0477 _refine_ls_wR_factor_all 0.1288 _refine_ls_wR_factor_obs 0.1226 _refine_ls_goodness_of_fit_all 1.045 _refine_ls_goodness_of_fit_obs 1.022 _refine_ls_restrained_S_all 1.045 _refine_ls_restrained_S_obs 1.022 _refine_ls_shift/esd_max 0.004 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni Ni 0.26561(3) 0.30581(5) 0.84913(3) 0.0657(3) Uani 1 d . . O1 O 0.1830(6) 0.2733(5) 1.0094(4) 0.0779(11) Uani 1 d . . N1 N 0.3691(9) 0.3238(5) 0.6797(5) 0.083(2) Uani 1 d . . O2 O 0.1658(6) 0.1347(4) 0.7951(3) 0.0835(10) Uani 1 d . . N2 N 0.4903(7) 0.2140(5) 0.8994(5) 0.0877(14) Uani 1 d . . O3 O 0.3526(4) 0.4818(4) 0.9047(3) 0.0748(9) Uani 1 d . . O4 O 0.0639(5) 0.3947(4) 0.7913(3) 0.0787(9) Uani 1 d . . C100 C 0.0263(10) 0.1941(6) 1.1578(6) 0.094(2) Uani 1 d . . H10A H 0.0813(10) 0.2622(6) 1.2002(6) 0.141 Uiso 1 calc R . H10B H 0.0474(10) 0.1114(6) 1.1948(6) 0.141 Uiso 1 calc R . H10C H -0.0847(10) 0.2113(6) 1.1567(6) 0.141 Uiso 1 calc R . C101 C 0.0821(8) 0.1901(5) 1.0335(6) 0.0714(15) Uani 1 d . . C102 C 0.0150(7) 0.0969(5) 0.9585(5) 0.0750(13) Uani 1 d . . H102 H -0.0653(7) 0.0452(5) 0.9862(5) 0.090 Uiso 1 calc R . C103 C 0.0594(7) 0.0754(5) 0.8450(5) 0.0759(14) Uani 1 d . . C104 C -0.0285(11) -0.0280(7) 0.7741(7) 0.112(2) Uani 1 d . . H10D H 0.0136(11) -0.0328(7) 0.6981(7) 0.168 Uiso 1 calc R . H10E H -0.1380(11) -0.0055(7) 0.7673(7) 0.168 Uiso 1 calc R . H10F H -0.0167(11) -0.1114(7) 0.8119(7) 0.168 Uiso 1 calc R . C200 C 0.3649(9) 0.7025(5) 0.9599(7) 0.092(2) Uani 1 d . . H20A H 0.4675(9) 0.6749(5) 0.9875(7) 0.138 Uiso 1 calc R . H20B H 0.3067(9) 0.7343(5) 1.0238(7) 0.138 Uiso 1 calc R . H20C H 0.3750(9) 0.7710(5) 0.9036(7) 0.138 Uiso 1 calc R . C201 C 0.2788(6) 0.5879(5) 0.9042(4) 0.0664(11) Uani 1 d . . C202 C 0.1272(7) 0.6075(5) 0.8583(5) 0.0748(13) Uani 1 d . . H202 H 0.0867(7) 0.6919(5) 0.8631(5) 0.090 Uiso 1 calc R . C203 C 0.0299(6) 0.5132(5) 0.8060(4) 0.0669(12) Uani 1 d . . C204 C -0.1345(7) 0.5550(7) 0.7622(6) 0.096(2) Uani 1 d . . H20D H -0.1887(7) 0.4811(7) 0.7282(6) 0.144 Uiso 1 calc R . H20E H -0.1257(7) 0.6226(7) 0.7048(6) 0.144 Uiso 1 calc R . H20F H -0.1922(7) 0.5877(7) 0.8260(6) 0.144 Uiso 1 calc R . C300 C 0.4263(12) 0.4517(9) 0.6574(8) 0.122(3) Uani 1 d . . H30G H 0.4881(12) 0.4820(9) 0.7235(8) 0.183 Uiso 1 calc R . H30H H 0.3391(12) 0.5099(9) 0.6429(8) 0.183 Uiso 1 calc R . H30I H 0.4903(12) 0.4495(9) 0.5906(8) 0.183 Uiso 1 calc R . C301 C 0.2744(13) 0.2671(13) 0.5873(6) 0.146(4) Uani 1 d . . H30L H 0.2407(13) 0.1814(13) 0.6098(6) 0.219 Uiso 1 calc R . H30M H 0.3351(13) 0.2605(13) 0.5190(6) 0.219 Uiso 1 calc R . H30N H 0.1841(13) 0.3214(13) 0.5711(6) 0.219 Uiso 1 calc R . C302 C 0.5114(15) 0.2321(15) 0.6925(9) 0.145(4) Uani 1 d . . H30O H 0.4764(15) 0.1430(15) 0.6781(9) 0.175 Uiso 1 calc R . H30P H 0.5852(15) 0.2544(15) 0.6335(9) 0.175 Uiso 1 calc R . C303 C 0.5905(10) 0.2370(12) 0.8021(9) 0.128(3) Uani 1 d . . H30J H 0.6394(10) 0.3224(12) 0.8116(9) 0.154 Uiso 1 calc R . H30K H 0.6738(10) 0.1721(12) 0.8041(9) 0.154 Uiso 1 calc R . C304 C 0.4726(11) 0.0735(7) 0.9215(7) 0.103(2) Uani 1 d . . H30A H 0.4061(11) 0.0609(7) 0.9860(7) 0.154 Uiso 1 calc R . H30B H 0.5741(11) 0.0356(7) 0.9392(7) 0.154 Uiso 1 calc R . H30C H 0.4261(11) 0.0319(7) 0.8538(7) 0.154 Uiso 1 calc R . C305 C 0.5625(10) 0.2723(9) 1.0045(9) 0.123(3) Uani 1 d . . H30D H 0.4964(10) 0.2570(9) 1.0688(9) 0.184 Uiso 1 calc R . H30E H 0.5747(10) 0.3648(9) 0.9932(9) 0.184 Uiso 1 calc R . H30F H 0.6638(10) 0.2333(9) 1.0204(9) 0.184 Uiso 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 Ni 0.0793(4) 0.0555(3) 0.0624(4) 0.0004(3) 0.0055(2) -0.0041(3) O1 0.098(3) 0.072(2) 0.064(2) -0.009(2) 0.008(2) -0.016(2) N1 0.100(4) 0.081(3) 0.069(3) 0.009(2) 0.017(3) 0.001(3) O2 0.119(3) 0.061(2) 0.072(2) -0.007(2) 0.011(2) -0.011(2) N2 0.093(3) 0.080(3) 0.090(3) 0.008(2) 0.004(3) 0.015(2) O3 0.073(2) 0.067(2) 0.084(2) 0.001(2) -0.004(2) -0.004(2) O4 0.080(2) 0.072(2) 0.084(2) 0.001(2) -0.004(2) -0.008(2) C100 0.113(5) 0.092(4) 0.077(4) 0.009(3) 0.020(3) -0.004(3) C101 0.080(4) 0.066(3) 0.068(3) 0.006(2) 0.006(3) 0.005(2) C102 0.083(3) 0.066(3) 0.076(3) -0.001(2) 0.003(3) -0.010(2) C103 0.096(3) 0.051(3) 0.079(3) -0.005(2) -0.010(3) -0.006(2) C104 0.140(6) 0.081(4) 0.114(5) -0.019(4) -0.017(4) -0.021(4) C200 0.103(4) 0.071(4) 0.101(5) -0.004(3) 0.001(4) -0.013(3) C201 0.076(3) 0.060(3) 0.063(2) 0.001(2) 0.004(2) -0.007(2) C202 0.087(3) 0.063(3) 0.075(3) 0.005(2) 0.006(2) 0.005(2) C203 0.072(3) 0.070(3) 0.059(2) 0.007(2) 0.009(2) -0.004(2) C204 0.078(3) 0.107(5) 0.101(4) 0.015(4) -0.010(3) 0.000(3) C300 0.161(7) 0.107(5) 0.102(5) 0.023(4) 0.045(5) -0.005(5) C301 0.173(9) 0.204(10) 0.061(4) -0.002(5) -0.001(5) -0.068(8) C302 0.146(9) 0.185(10) 0.110(8) 0.030(7) 0.052(7) 0.047(8) C303 0.098(5) 0.151(7) 0.139(8) 0.049(6) 0.031(5) 0.042(5) C304 0.133(5) 0.078(4) 0.096(4) 0.011(3) -0.006(4) 0.028(4) C305 0.117(5) 0.108(5) 0.140(7) -0.012(5) -0.051(5) 0.025(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 Ni O1 2.029(4) . ? Ni O4 2.030(4) . ? Ni O2 2.030(4) . ? Ni O3 2.037(4) . ? Ni N1 2.180(6) . ? Ni N2 2.187(5) . ? O1 C101 1.246(8) . ? N1 C300 1.421(10) . ? N1 C301 1.432(10) . ? N1 C302 1.533(13) . ? O2 C103 1.247(7) . ? N2 C303 1.454(10) . ? N2 C305 1.462(10) . ? N2 C304 1.466(8) . ? O3 C201 1.253(6) . ? O4 C203 1.257(7) . ? C100 C101 1.527(10) . ? C101 C102 1.393(8) . ? C102 C103 1.393(9) . ? C103 C104 1.515(8) . ? C200 C201 1.509(8) . ? C201 C202 1.389(8) . ? C202 C203 1.392(8) . ? C203 C204 1.529(8) . ? C302 C303 1.408(14) . ? 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 O1 Ni O4 93.1(2) . . ? O1 Ni O2 89.0(2) . . ? O4 Ni O2 86.9(2) . . ? O1 Ni O3 89.6(2) . . ? O4 Ni O3 90.04(14) . . ? O2 Ni O3 176.6(2) . . ? O1 Ni N1 174.3(3) . . ? O4 Ni N1 92.0(2) . . ? O2 Ni N1 88.6(2) . . ? O3 Ni N1 93.0(2) . . ? O1 Ni N2 91.1(2) . . ? O4 Ni N2 175.8(2) . . ? O2 Ni N2 93.6(2) . . ? O3 Ni N2 89.5(2) . . ? N1 Ni N2 83.9(2) . . ? C101 O1 Ni 125.4(4) . . ? C300 N1 C301 115.0(8) . . ? C300 N1 C302 107.7(9) . . ? C301 N1 C302 104.1(9) . . ? C300 N1 Ni 113.1(5) . . ? C301 N1 Ni 113.4(5) . . ? C302 N1 Ni 102.0(5) . . ? C103 O2 Ni 125.3(3) . . ? C303 N2 C305 109.4(8) . . ? C303 N2 C304 111.1(7) . . ? C305 N2 C304 107.3(6) . . ? C303 N2 Ni 105.0(4) . . ? C305 N2 Ni 112.3(4) . . ? C304 N2 Ni 111.8(5) . . ? C201 O3 Ni 125.9(3) . . ? C203 O4 Ni 125.6(3) . . ? O1 C101 C102 126.6(6) . . ? O1 C101 C100 115.6(5) . . ? C102 C101 C100 117.7(6) . . ? C101 C102 C103 124.8(5) . . ? O2 C103 C102 125.8(5) . . ? O2 C103 C104 116.2(5) . . ? C102 C103 C104 118.0(6) . . ? O3 C201 C202 125.7(5) . . ? O3 C201 C200 115.7(5) . . ? C202 C201 C200 118.5(5) . . ? C201 C202 C203 126.3(5) . . ? O4 C203 C202 126.1(5) . . ? O4 C203 C204 115.9(5) . . ? C202 C203 C204 118.0(5) . . ? C303 C302 N1 114.4(9) . . ? C302 C303 N2 114.3(8) . . ? _refine_diff_density_max 0.424 _refine_diff_density_min -0.238 _refine_diff_density_rms 0.057