# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Stephen Holmes' _publ_contact_author_address ; Chemistry University of Kentucky 15 Chemistry-Physics Bldg. Lexington KY 40506-0055 UNITED STATES OF AMERICA ; _publ_contact_author_email SMHOLM2@UKY.EDU _publ_section_title ; Syntheses, Structures, and Magnetic Characterization of Dicyanometalate(II) Building Blocks: [NEt4][(Tp*)MII(CN)2] [MII = Cr, Co, Ni; Tp* = hydridotris(3,5-diemethylpyrazolyl)borate] ; loop_ _publ_author_name 'Stephen Holmes' 'Rodolphe Clerac' 'Dongfeng Li.' 'Sean Parkin' 'Chad Ruschman' # Attachment '1_new.cif' # CCDC 610652 data_x05077_NEt4Tp*Cr(CN)2.0.5CH3CN.0.5Et2O _database_code_depnum_ccdc_archive 'CCDC 610652' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H48.50 B Cr N9.50 O0.50' _chemical_formula_weight 589.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 10.1192(3) _cell_length_b 13.9716(4) _cell_length_c 24.4089(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.565(2) _cell_angle_gamma 90.00 _cell_volume 3449.68(17) _cell_formula_units_Z 4 _cell_measurement_temperature 90.0(2) _cell_measurement_reflns_used 6076 _cell_measurement_theta_min 3.62 _cell_measurement_theta_max 67.63 _exptl_crystal_description needle _exptl_crystal_colour purple-orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.134 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 2.978 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5873 _exptl_absorpt_correction_T_max 0.9293 _exptl_absorpt_process_details 'Bruker SAINT' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90.0(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Proteum CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40970 _diffrn_reflns_av_R_equivalents 0.0908 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 4.37 _diffrn_reflns_theta_max 68.10 _reflns_number_total 6213 _reflns_number_gt 4925 _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^)+(0.1309P)^2^+5.9795P] 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 6213 _refine_ls_number_parameters 368 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0927 _refine_ls_R_factor_gt 0.0761 _refine_ls_wR_factor_ref 0.2234 _refine_ls_wR_factor_gt 0.2104 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Cr1 Cr 0.36490(6) 0.48831(4) 0.16851(2) 0.0266(2) Uani 1 1 d . . . B1 B 0.4038(4) 0.6646(3) 0.08770(17) 0.0294(9) Uani 1 1 d . . . H1 H 0.4240 0.7272 0.0611 0.035 Uiso 1 1 d R . . N1 N 0.5160(3) 0.5064(2) 0.11190(13) 0.0288(7) Uani 1 1 d . . . N2 N 0.5063(3) 0.5848(2) 0.07757(12) 0.0288(7) Uani 1 1 d . . . N3 N 0.4076(3) 0.6320(2) 0.19000(13) 0.0315(7) Uani 1 1 d . . . N4 N 0.4195(3) 0.6973(2) 0.14818(13) 0.0312(7) Uani 1 1 d . . . N5 N 0.2254(3) 0.5433(2) 0.10276(12) 0.0284(7) Uani 1 1 d . . . N6 N 0.2625(3) 0.6260(2) 0.07729(12) 0.0294(7) Uani 1 1 d . . . N7 N 0.1687(4) 0.4634(3) 0.27073(17) 0.0534(11) Uani 1 1 d . . . N8 N 0.3239(4) 0.2633(3) 0.13875(15) 0.0402(8) Uani 1 1 d . . . C1 C 0.6568(4) 0.3629(3) 0.12355(18) 0.0379(9) Uani 1 1 d . . . H1A H 0.6523 0.3720 0.1633 0.057 Uiso 1 1 calc R . . H1B H 0.7473 0.3459 0.1141 0.057 Uiso 1 1 calc R . . H1C H 0.5964 0.3114 0.1121 0.057 Uiso 1 1 calc R . . C2 C 0.6176(4) 0.4534(3) 0.09498(16) 0.0303(8) Uani 1 1 d . . . C3 C 0.6733(4) 0.4967(3) 0.04956(17) 0.0332(9) Uani 1 1 d . . . H3A H 0.7461 0.4739 0.0295 0.040 Uiso 1 1 calc R . . C4 C 0.6014(4) 0.5795(3) 0.03951(15) 0.0319(9) Uani 1 1 d . . . C5 C 0.6200(4) 0.6531(3) -0.00350(16) 0.0398(10) Uani 1 1 d . . . H5A H 0.5367 0.6625 -0.0242 0.060 Uiso 1 1 calc R . . H5B H 0.6885 0.6318 -0.0284 0.060 Uiso 1 1 calc R . . H5C H 0.6472 0.7136 0.0137 0.060 Uiso 1 1 calc R . . C6 C 0.4326(5) 0.6295(3) 0.29165(17) 0.0428(10) Uani 1 1 d . . . H6A H 0.4648 0.5637 0.2879 0.064 Uiso 1 1 calc R . . H6B H 0.3421 0.6285 0.3049 0.064 Uiso 1 1 calc R . . H6C H 0.4898 0.6643 0.3179 0.064 Uiso 1 1 calc R . . C7 C 0.4343(4) 0.6785(3) 0.23702(16) 0.0337(9) Uani 1 1 d . . . C8 C 0.4629(4) 0.7741(3) 0.22537(17) 0.0392(10) Uani 1 1 d . . . H8A H 0.4846 0.8231 0.2511 0.047 Uiso 1 1 calc R . . C9 C 0.4532(4) 0.7832(3) 0.16965(17) 0.0356(9) Uani 1 1 d . . . C10 C 0.4733(5) 0.8705(3) 0.1354(2) 0.0490(11) Uani 1 1 d . . . H10A H 0.5383 0.8566 0.1074 0.073 Uiso 1 1 calc R . . H10B H 0.5057 0.9230 0.1587 0.073 Uiso 1 1 calc R . . H10C H 0.3892 0.8890 0.1175 0.073 Uiso 1 1 calc R . . C11 C 0.0333(4) 0.4355(3) 0.10401(18) 0.0384(9) Uani 1 1 d . . . H11A H 0.0457 0.4294 0.1438 0.058 Uiso 1 1 calc R . . H11B H 0.0698 0.3791 0.0860 0.058 Uiso 1 1 calc R . . H11C H -0.0612 0.4407 0.0947 0.058 Uiso 1 1 calc R . . C12 C 0.1031(4) 0.5233(3) 0.08485(16) 0.0314(8) Uani 1 1 d . . . C13 C 0.0592(4) 0.5940(3) 0.04810(16) 0.0354(9) Uani 1 1 d . . . H13A H -0.0245 0.5972 0.0296 0.042 Uiso 1 1 calc R . . C14 C 0.1618(4) 0.6583(3) 0.04415(16) 0.0333(9) Uani 1 1 d . . . C15 C 0.1720(5) 0.7469(3) 0.01080(19) 0.0460(11) Uani 1 1 d . . . H15A H 0.1851 0.8021 0.0351 0.069 Uiso 1 1 calc R . . H15B H 0.0905 0.7555 -0.0113 0.069 Uiso 1 1 calc R . . H15C H 0.2472 0.7414 -0.0135 0.069 Uiso 1 1 calc R . . C16 C 0.2395(4) 0.4714(3) 0.23541(18) 0.0374(9) Uani 1 1 d . . . C17 C 0.3423(4) 0.3415(3) 0.15002(15) 0.0324(9) Uani 1 1 d . . . N9 N 0.9194(4) 0.6819(4) 0.2245(2) 0.0705(15) Uani 1 1 d . . . C18 C 0.8888(7) 0.5735(5) 0.2303(4) 0.090(2) Uani 1 1 d . . . H18A H 0.8901 0.5439 0.1935 0.108 Uiso 1 1 calc R . . H18B H 0.9607 0.5437 0.2528 0.108 Uiso 1 1 calc R . . C19 C 0.7582(7) 0.5498(6) 0.2559(4) 0.101(3) Uani 1 1 d . . . H19A H 0.7538 0.4808 0.2631 0.152 Uiso 1 1 calc R . . H19B H 0.6855 0.5682 0.2308 0.152 Uiso 1 1 calc R . . H19C H 0.7508 0.5848 0.2905 0.152 Uiso 1 1 calc R . . C20 C 0.8094(5) 0.7336(5) 0.1941(3) 0.078(2) Uani 1 1 d . . . H20A H 0.7285 0.7296 0.2159 0.094 Uiso 1 1 calc R . . H20B H 0.8334 0.8020 0.1912 0.094 Uiso 1 1 calc R . . C21 C 0.7790(7) 0.6958(6) 0.1380(3) 0.095(3) Uani 1 1 d . . . H21A H 0.6959 0.7237 0.1240 0.143 Uiso 1 1 calc R . . H21B H 0.7704 0.6260 0.1396 0.143 Uiso 1 1 calc R . . H21C H 0.8506 0.7129 0.1137 0.143 Uiso 1 1 calc R . . C22 C 0.9296(6) 0.7273(5) 0.2810(3) 0.0765(19) Uani 1 1 d . . . H22A H 0.8463 0.7150 0.3001 0.092 Uiso 1 1 calc R . . H22B H 0.9379 0.7975 0.2765 0.092 Uiso 1 1 calc R . . C23 C 1.0444(9) 0.6923(6) 0.3171(3) 0.098(3) Uani 1 1 d . . . H23A H 1.0386 0.7209 0.3537 0.146 Uiso 1 1 calc R . . H23B H 1.1280 0.7111 0.3009 0.146 Uiso 1 1 calc R . . H23C H 1.0406 0.6225 0.3202 0.146 Uiso 1 1 calc R . . C24 C 1.0493(5) 0.6897(5) 0.1962(3) 0.0716(19) Uani 1 1 d . . . H24A H 1.1172 0.6539 0.2177 0.086 Uiso 1 1 calc R . . H24B H 1.0403 0.6588 0.1598 0.086 Uiso 1 1 calc R . . C25 C 1.0953(6) 0.7885(6) 0.1888(3) 0.089(2) Uani 1 1 d . . . H25A H 1.1784 0.7881 0.1691 0.133 Uiso 1 1 calc R . . H25B H 1.1098 0.8186 0.2247 0.133 Uiso 1 1 calc R . . H25C H 1.0285 0.8247 0.1677 0.133 Uiso 1 1 calc R . . N10 N 0.838(2) 0.858(2) 0.9560(10) 0.173(9) Uiso 0.50 1 d P A 1 C26 C 0.827(4) 0.935(3) 0.9413(15) 0.196(13) Uiso 0.50 1 d P A 1 C27 C 0.883(4) 1.008(2) 0.9119(15) 0.200(14) Uiso 0.50 1 d P A 1 H27A H 0.8486 1.0695 0.9245 0.300 Uiso 0.50 1 calc PR A 1 H27B H 0.8611 0.9999 0.8728 0.300 Uiso 0.50 1 calc PR A 1 H27C H 0.9793 1.0066 0.9176 0.300 Uiso 0.50 1 calc PR A 1 C28 C 0.859(5) 0.951(3) 1.0762(19) 0.27(2) Uiso 0.50 1 d P B 2 H28A H 0.9361 0.9138 1.0663 0.404 Uiso 0.50 1 calc PR B 2 H28B H 0.8200 0.9240 1.1091 0.404 Uiso 0.50 1 calc PR B 2 H28C H 0.8852 1.0177 1.0835 0.404 Uiso 0.50 1 calc PR B 2 C29 C 0.759(5) 0.949(4) 1.030(2) 0.27(2) Uiso 0.50 1 d P B 2 H29A H 0.7654 0.8807 1.0203 0.322 Uiso 0.50 1 d PR B 2 H29B H 0.8079 0.9829 1.0014 0.322 Uiso 0.50 1 d PR B 2 O1 O 0.58(2) 0.998(18) 1.015(12) 0.3(5) Uiso 0.50 1 d P . 2 C30 C 0.58(3) 1.00(3) 1.015(18) 0.3(7) Uiso 0.50 1 d P . 2 H30A H 0.5165 0.9518 1.0207 0.321 Uiso 0.50 1 d PR . 2 H30B H 0.5760 1.0211 0.9780 0.321 Uiso 0.50 1 d PR . 2 C31 C 0.558(5) 1.087(3) 1.0549(18) 0.260(19) Uiso 0.50 1 d P C 2 H31A H 0.6433 1.0944 1.0741 0.390 Uiso 0.50 1 d PR C 2 H31B H 0.5360 1.1467 1.0352 0.390 Uiso 0.50 1 d PR C 2 H31C H 0.4891 1.0740 1.0814 0.390 Uiso 0.50 1 d PR C 2 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 Cr1 0.0256(4) 0.0268(3) 0.0277(3) 0.0006(2) 0.0041(2) -0.0009(2) B1 0.031(2) 0.026(2) 0.032(2) 0.0012(16) 0.0034(17) -0.0038(17) N1 0.0261(17) 0.0303(16) 0.0303(16) 0.0015(12) 0.0043(13) -0.0034(13) N2 0.0270(17) 0.0320(17) 0.0275(15) -0.0006(12) 0.0033(12) -0.0045(13) N3 0.0304(17) 0.0343(18) 0.0301(16) -0.0009(13) 0.0032(13) -0.0037(14) N4 0.0323(18) 0.0286(17) 0.0329(17) -0.0022(13) 0.0056(13) -0.0045(13) N5 0.0270(17) 0.0279(16) 0.0306(16) 0.0012(12) 0.0033(13) -0.0015(13) N6 0.0328(18) 0.0263(16) 0.0292(16) 0.0007(12) 0.0027(13) 0.0002(13) N7 0.064(3) 0.049(2) 0.049(2) -0.0024(18) 0.027(2) -0.007(2) N8 0.046(2) 0.031(2) 0.044(2) 0.0003(15) 0.0059(16) -0.0057(16) C1 0.028(2) 0.041(2) 0.045(2) 0.0016(18) 0.0069(17) 0.0034(17) C2 0.0212(19) 0.034(2) 0.035(2) -0.0029(16) 0.0022(15) -0.0025(15) C3 0.028(2) 0.037(2) 0.035(2) -0.0066(16) 0.0054(16) -0.0023(16) C4 0.027(2) 0.041(2) 0.0280(18) -0.0028(15) 0.0026(15) -0.0084(16) C5 0.040(2) 0.048(3) 0.032(2) 0.0012(18) 0.0073(17) -0.0081(19) C6 0.048(3) 0.049(3) 0.031(2) -0.0074(18) 0.0012(18) -0.006(2) C7 0.031(2) 0.036(2) 0.034(2) -0.0060(16) 0.0033(16) -0.0011(16) C8 0.039(2) 0.037(2) 0.041(2) -0.0119(17) 0.0059(18) -0.0058(18) C9 0.038(2) 0.028(2) 0.040(2) -0.0046(16) 0.0058(17) -0.0043(17) C10 0.063(3) 0.034(2) 0.050(3) -0.0029(19) 0.003(2) -0.010(2) C11 0.029(2) 0.042(2) 0.045(2) 0.0032(18) 0.0031(17) -0.0070(18) C12 0.029(2) 0.033(2) 0.0318(19) -0.0011(15) 0.0049(16) 0.0002(16) C13 0.027(2) 0.041(2) 0.038(2) -0.0001(17) 0.0005(16) 0.0054(17) C14 0.030(2) 0.035(2) 0.034(2) -0.0026(16) 0.0008(16) 0.0048(17) C15 0.048(3) 0.043(3) 0.046(2) 0.009(2) -0.003(2) 0.003(2) C16 0.042(2) 0.031(2) 0.040(2) -0.0019(16) 0.0066(19) -0.0006(18) C17 0.026(2) 0.041(2) 0.0305(19) 0.0053(16) 0.0041(15) -0.0013(17) N9 0.031(2) 0.069(3) 0.111(4) -0.057(3) 0.003(2) 0.010(2) C18 0.055(4) 0.068(4) 0.147(7) -0.042(4) -0.003(4) 0.008(3) C19 0.065(5) 0.080(5) 0.158(8) -0.013(5) 0.005(5) -0.003(4) C20 0.032(3) 0.080(4) 0.122(5) -0.050(4) -0.001(3) 0.016(3) C21 0.069(4) 0.095(5) 0.119(6) -0.053(5) -0.024(4) 0.017(4) C22 0.061(4) 0.070(4) 0.100(5) -0.043(4) 0.027(3) 0.008(3) C23 0.118(7) 0.083(5) 0.092(5) -0.036(4) 0.002(5) 0.029(5) C24 0.035(3) 0.096(5) 0.084(4) -0.049(4) 0.002(3) 0.013(3) C25 0.041(3) 0.113(6) 0.114(6) -0.020(5) 0.020(3) 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 Cr1 N1 2.104(3) . ? Cr1 C16 2.108(4) . ? Cr1 C17 2.111(4) . ? Cr1 N3 2.116(3) . ? Cr1 N5 2.244(3) . ? B1 N6 1.543(5) . ? B1 N2 1.547(5) . ? B1 N4 1.549(5) . ? N1 C2 1.341(5) . ? N1 N2 1.381(4) . ? N2 C4 1.358(5) . ? N3 C7 1.340(5) . ? N3 N4 1.377(4) . ? N4 C9 1.350(5) . ? N5 C12 1.331(5) . ? N5 N6 1.370(4) . ? N6 C14 1.360(5) . ? N7 C16 1.142(6) . ? N8 C17 1.141(5) . ? C1 C2 1.493(6) . ? C2 C3 1.395(6) . ? C3 C4 1.385(6) . ? C4 C5 1.486(6) . ? C6 C7 1.499(6) . ? C7 C8 1.398(6) . ? C8 C9 1.367(6) . ? C9 C10 1.496(6) . ? C11 C12 1.496(6) . ? C12 C13 1.399(6) . ? C13 C14 1.378(6) . ? C14 C15 1.486(6) . ? N9 C20 1.505(8) . ? N9 C24 1.506(7) . ? N9 C22 1.519(7) . ? N9 C18 1.553(9) . ? C18 C19 1.514(11) . ? C20 C21 1.491(9) . ? C22 C23 1.520(10) . ? C24 C25 1.470(10) . ? N10 C26 1.13(4) . ? C26 C27 1.38(4) . ? C28 C29 1.49(5) . ? C29 C30 1.9(3) . ? C29 O1 1.9(3) . ? O1 C31 1.6(3) . ? O1 C30 1.84(12) 3_677 ? C30 C31 1.6(4) . ? C30 C30 1.8(7) 3_677 ? C30 O1 1.84(11) 3_677 ? 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 N1 Cr1 C16 170.27(15) . . ? N1 Cr1 C17 93.03(13) . . ? C16 Cr1 C17 89.58(15) . . ? N1 Cr1 N3 84.36(12) . . ? C16 Cr1 N3 92.14(14) . . ? C17 Cr1 N3 174.08(14) . . ? N1 Cr1 N5 86.75(12) . . ? C16 Cr1 N5 102.26(15) . . ? C17 Cr1 N5 96.74(13) . . ? N3 Cr1 N5 88.43(12) . . ? N6 B1 N2 110.1(3) . . ? N6 B1 N4 109.3(3) . . ? N2 B1 N4 108.3(3) . . ? C2 N1 N2 107.1(3) . . ? C2 N1 Cr1 135.5(3) . . ? N2 N1 Cr1 116.9(2) . . ? C4 N2 N1 109.4(3) . . ? C4 N2 B1 129.7(3) . . ? N1 N2 B1 120.8(3) . . ? C7 N3 N4 107.1(3) . . ? C7 N3 Cr1 135.0(3) . . ? N4 N3 Cr1 117.8(2) . . ? C9 N4 N3 109.1(3) . . ? C9 N4 B1 130.5(3) . . ? N3 N4 B1 120.2(3) . . ? C12 N5 N6 106.9(3) . . ? C12 N5 Cr1 136.4(3) . . ? N6 N5 Cr1 116.1(2) . . ? C14 N6 N5 109.9(3) . . ? C14 N6 B1 131.1(3) . . ? N5 N6 B1 118.9(3) . . ? N1 C2 C3 109.6(4) . . ? N1 C2 C1 121.3(3) . . ? C3 C2 C1 129.1(4) . . ? C4 C3 C2 106.3(3) . . ? N2 C4 C3 107.7(3) . . ? N2 C4 C5 123.5(4) . . ? C3 C4 C5 128.8(4) . . ? N3 C7 C8 109.1(4) . . ? N3 C7 C6 122.3(4) . . ? C8 C7 C6 128.6(4) . . ? C9 C8 C7 106.4(4) . . ? N4 C9 C8 108.3(4) . . ? N4 C9 C10 123.0(4) . . ? C8 C9 C10 128.7(4) . . ? N5 C12 C13 109.8(3) . . ? N5 C12 C11 120.8(4) . . ? C13 C12 C11 129.4(4) . . ? C14 C13 C12 106.2(4) . . ? N6 C14 C13 107.2(4) . . ? N6 C14 C15 122.7(4) . . ? C13 C14 C15 130.1(4) . . ? N7 C16 Cr1 178.0(4) . . ? N8 C17 Cr1 176.4(4) . . ? C20 N9 C24 112.5(6) . . ? C20 N9 C22 106.1(4) . . ? C24 N9 C22 110.4(4) . . ? C20 N9 C18 111.5(5) . . ? C24 N9 C18 106.9(4) . . ? C22 N9 C18 109.5(6) . . ? C19 C18 N9 115.5(5) . . ? C21 C20 N9 114.5(5) . . ? N9 C22 C23 115.1(5) . . ? C25 C24 N9 114.1(5) . . ? N10 C26 C27 146(4) . . ? C28 C29 C30 138(10) . . ? C28 C29 O1 138(9) . . ? C30 C29 O1 0(10) . . ? C31 O1 C30 93(10) . 3_677 ? C31 O1 C29 109(10) . . ? C30 O1 C29 157(5) 3_677 . ? C31 C30 C30 93(10) . 3_677 ? C31 C30 O1 93(10) . 3_677 ? C30 C30 O1 0(10) 3_677 3_677 ? C31 C30 C29 109(10) . . ? C30 C30 C29 157(10) 3_677 . ? O1 C30 C29 157(10) 3_677 . ? C30 C31 O1 0(10) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 68.10 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.092 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.094 # Attachment '2_new.cif' # CCDC 610653 data_k05042_NEt4Tp*Co(CN)2.CH3CN.0.5Et2O _database_code_depnum_ccdc_archive 'CCDC 610653' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H50 B Co N10 O0.50' _chemical_formula_weight 616.53 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' O O 0.0106 0.0060 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 9.9894(2) _cell_length_b 13.7890(3) _cell_length_c 24.3416(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.2557(10) _cell_angle_gamma 90.00 _cell_volume 3347.49(13) _cell_formula_units_Z 4 _cell_measurement_temperature 90.0(2) _cell_measurement_reflns_used 7356 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.223 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.549 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8103 _exptl_absorpt_correction_T_max 0.8526 _exptl_absorpt_process_details 'Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90.0(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 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\w scans at fixed \c = 55\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13593 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0759 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7636 _reflns_number_gt 4767 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL (Sheldrick, 1994)' _computing_publication_material ; SHELX97-2 (Sheldrick, 1997) and local procedures ; _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^)+(0.0769P)^2^+3.1597P] 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 7636 _refine_ls_number_parameters 401 _refine_ls_number_restraints 58 _refine_ls_R_factor_all 0.1144 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1718 _refine_ls_wR_factor_gt 0.1503 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.080 _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 Co1 Co 0.36863(4) 1.00049(3) 0.165525(16) 0.01917(14) Uani 1 1 d . . . B1 B 0.4063(4) 0.8316(3) 0.08540(15) 0.0230(8) Uani 1 1 d . . . H1 H 0.4225 0.7767 0.0598 0.028 Uiso 1 1 calc R . . N1 N 0.4201(3) 0.8668(2) 0.18689(10) 0.0220(6) Uani 1 1 d . . . N2 N 0.4282(3) 0.79864(19) 0.14576(10) 0.0220(6) Uani 1 1 d . . . N3 N 0.5084(3) 0.99414(19) 0.11184(10) 0.0192(6) Uani 1 1 d . . . N4 N 0.5063(3) 0.91484(19) 0.07687(10) 0.0205(6) Uani 1 1 d . . . N5 N 0.2275(3) 0.95064(19) 0.10480(10) 0.0204(6) Uani 1 1 d . . . N6 N 0.2631(3) 0.86993(19) 0.07601(10) 0.0200(6) Uani 1 1 d . . . N7 N 0.3107(3) 1.2143(2) 0.14158(11) 0.0267(7) Uani 1 1 d . . . N8 N 0.1772(3) 1.0098(2) 0.25850(12) 0.0288(7) Uani 1 1 d . . . C1 C 0.4649(4) 0.8749(3) 0.28826(14) 0.0373(9) Uani 1 1 d . . . H1A H 0.5018 0.9399 0.2833 0.056 Uiso 1 1 calc R . . H1B H 0.5230 0.8388 0.3149 0.056 Uiso 1 1 calc R . . H1C H 0.3749 0.8802 0.3020 0.056 Uiso 1 1 calc R . . C2 C 0.4573(3) 0.8226(3) 0.23447(13) 0.0276(8) Uani 1 1 d . . . C3 C 0.4904(4) 0.7261(3) 0.22392(14) 0.0303(8) Uani 1 1 d . . . H3A H 0.5208 0.6789 0.2502 0.036 Uiso 1 1 calc R . . C4 C 0.4702(3) 0.7129(2) 0.16818(14) 0.0252(8) Uani 1 1 d . . . C5 C 0.4883(4) 0.6239(3) 0.13449(15) 0.0359(9) Uani 1 1 d . . . H5A H 0.5294 0.6414 0.1003 0.054 Uiso 1 1 calc R . . H5B H 0.4008 0.5937 0.1258 0.054 Uiso 1 1 calc R . . H5C H 0.5465 0.5781 0.1553 0.054 Uiso 1 1 calc R . . C6 C 0.6435(3) 1.1428(2) 0.12749(14) 0.0264(8) Uani 1 1 d . . . H6A H 0.6267 1.1351 0.1665 0.040 Uiso 1 1 calc R . . H6B H 0.5875 1.1953 0.1118 0.040 Uiso 1 1 calc R . . H6C H 0.7382 1.1584 0.1237 0.040 Uiso 1 1 calc R . . C7 C 0.6101(3) 1.0509(2) 0.09782(13) 0.0225(7) Uani 1 1 d . . . C8 C 0.6726(3) 1.0088(2) 0.05384(13) 0.0224(7) Uani 1 1 d . . . H8A H 0.7470 1.0341 0.0359 0.027 Uiso 1 1 calc R . . C9 C 0.6055(3) 0.9236(2) 0.04152(12) 0.0207(7) Uani 1 1 d . . . C10 C 0.6297(3) 0.8509(3) -0.00263(13) 0.0258(8) Uani 1 1 d . . . H10A H 0.5448 0.8360 -0.0230 0.039 Uiso 1 1 calc R . . H10B H 0.6671 0.7915 0.0142 0.039 Uiso 1 1 calc R . . H10C H 0.6931 0.8778 -0.0279 0.039 Uiso 1 1 calc R . . C11 C 0.0339(3) 1.0612(2) 0.10842(14) 0.0257(8) Uani 1 1 d . . . H11A H 0.0521 1.0657 0.1483 0.039 Uiso 1 1 calc R . . H11B H -0.0629 1.0548 0.1002 0.039 Uiso 1 1 calc R . . H11C H 0.0665 1.1198 0.0908 0.039 Uiso 1 1 calc R . . C12 C 0.1034(3) 0.9749(2) 0.08707(13) 0.0211(7) Uani 1 1 d . . . C13 C 0.0572(3) 0.9085(2) 0.04627(13) 0.0231(7) Uani 1 1 d . . . H13A H -0.0278 0.9088 0.0267 0.028 Uiso 1 1 calc R . . C14 C 0.1597(3) 0.8432(2) 0.04040(13) 0.0233(7) Uani 1 1 d . . . C15 C 0.1683(4) 0.7577(3) 0.00331(14) 0.0312(8) Uani 1 1 d . . . H15A H 0.2485 0.7633 -0.0178 0.047 Uiso 1 1 calc R . . H15B H 0.0884 0.7555 -0.0220 0.047 Uiso 1 1 calc R . . H15C H 0.1735 0.6982 0.0253 0.047 Uiso 1 1 calc R . . C16 C 0.3360(3) 1.1345(3) 0.15130(13) 0.0225(7) Uani 1 1 d . . . C17 C 0.2513(3) 1.0079(2) 0.22373(13) 0.0226(7) Uani 1 1 d . . . N9 N 0.9387(3) 0.7762(2) 0.20817(12) 0.0317(7) Uani 1 1 d . . . C18 C 0.7787(5) 0.9185(4) 0.2078(3) 0.0718(17) Uani 1 1 d . . . H18A H 0.7700 0.9869 0.1972 0.108 Uiso 1 1 calc R . . H18B H 0.7648 0.9118 0.2471 0.108 Uiso 1 1 calc R . . H18C H 0.7115 0.8801 0.1866 0.108 Uiso 1 1 calc R . . C19 C 0.9161(4) 0.8831(3) 0.19633(17) 0.0427(10) Uani 1 1 d . . . H19A H 0.9830 0.9211 0.2189 0.051 Uiso 1 1 calc R . . H19B H 0.9319 0.8955 0.1572 0.051 Uiso 1 1 calc R . . C20 C 1.0086(5) 0.8029(3) 0.30923(17) 0.0545(13) Uani 1 1 d . . . H20A H 0.9832 0.7865 0.3464 0.082 Uiso 1 1 calc R . . H20B H 1.0016 0.8731 0.3037 0.082 Uiso 1 1 calc R . . H20C H 1.1012 0.7822 0.3047 0.082 Uiso 1 1 calc R . . C21 C 0.9160(4) 0.7516(3) 0.26741(15) 0.0369(9) Uani 1 1 d . . . H21A H 0.9268 0.6808 0.2725 0.044 Uiso 1 1 calc R . . H21B H 0.8222 0.7681 0.2749 0.044 Uiso 1 1 calc R . . C22 C 1.1287(5) 0.6527(4) 0.2092(3) 0.0805(18) Uani 1 1 d . . . H22A H 1.2239 0.6457 0.2022 0.121 Uiso 1 1 calc R . . H22B H 1.0760 0.6061 0.1865 0.121 Uiso 1 1 calc R . . H22C H 1.1159 0.6402 0.2482 0.121 Uiso 1 1 calc R . . C23 C 1.0829(4) 0.7551(4) 0.19469(18) 0.0501(12) Uani 1 1 d . . . H23A H 1.0919 0.7658 0.1549 0.060 Uiso 1 1 calc R . . H23B H 1.1428 0.8017 0.2149 0.060 Uiso 1 1 calc R . . C24 C 0.8444(5) 0.7294(4) 0.11136(17) 0.0638(15) Uani 1 1 d . . . H24A H 0.7850 0.6822 0.0922 0.096 Uiso 1 1 calc R . . H24B H 0.9361 0.7205 0.0999 0.096 Uiso 1 1 calc R . . H24C H 0.8139 0.7952 0.1021 0.096 Uiso 1 1 calc R . . C25 C 0.8416(4) 0.7139(3) 0.17346(16) 0.0418(10) Uani 1 1 d . . . H25A H 0.7496 0.7270 0.1847 0.050 Uiso 1 1 calc R . . H25B H 0.8617 0.6449 0.1816 0.050 Uiso 1 1 calc R . . N10 N 0.0905(8) 0.5401(6) 0.0791(3) 0.138(2) Uani 1 1 d U . . C26 C 0.1314(9) 0.4664(5) 0.0645(3) 0.106(3) Uani 1 1 d . . . C27 C 0.1794(8) 0.3786(4) 0.0467(3) 0.095(2) Uani 1 1 d . . . H27A H 0.1292 0.3593 0.0127 0.143 Uiso 1 1 calc R . . H27B H 0.1686 0.3292 0.0750 0.143 Uiso 1 1 calc R . . H27C H 0.2746 0.3851 0.0396 0.143 Uiso 1 1 calc R . . O1 O 0.5706(5) 0.5003(4) 0.0144(2) 0.1033(17) Uani 0.50 1 d PU . 1 C28 C 0.7477(12) 0.4367(6) 0.0857(4) 0.069(3) Uani 0.50 1 d PU A 1 H28A H 0.7731 0.3775 0.1060 0.103 Uiso 0.50 1 calc PR A 1 H28B H 0.7438 0.4911 0.1114 0.103 Uiso 0.50 1 calc PR A 1 H28C H 0.8143 0.4504 0.0587 0.103 Uiso 0.50 1 calc PR A 1 C29 C 0.6041(18) 0.4219(17) 0.0546(9) 0.086(3) Uani 0.50 1 d PU A 1 H29A H 0.6026 0.3589 0.0351 0.104 Uiso 0.50 1 calc PR A 1 H29B H 0.5348 0.4198 0.0821 0.104 Uiso 0.50 1 calc PR A 1 C30 C 0.5518(14) 0.4114(15) 0.0509(8) 0.069(4) Uani 0.50 1 d PU B 2 H30A H 0.6358 0.3975 0.0722 0.104 Uiso 0.50 1 calc PR B 2 H30B H 0.5267 0.3554 0.0278 0.104 Uiso 0.50 1 calc PR B 2 H30C H 0.4808 0.4244 0.0761 0.104 Uiso 0.50 1 calc PR B 2 C31 C 0.5706(5) 0.5003(4) 0.0144(2) 0.1033(17) Uani 0.50 1 d PU . 2 H31A H 0.6419 0.4906 -0.0117 0.124 Uiso 0.50 1 calc PR . 2 H31B H 0.5884 0.5601 0.0361 0.124 Uiso 0.50 1 calc PR . 2 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 Co1 0.0186(2) 0.0196(2) 0.0193(2) -0.00092(18) 0.00090(15) 0.0022(2) B1 0.027(2) 0.0185(19) 0.0237(19) -0.0006(15) 0.0019(15) 0.0029(17) N1 0.0228(15) 0.0215(15) 0.0219(14) -0.0012(11) 0.0035(11) 0.0052(12) N2 0.0264(16) 0.0169(14) 0.0228(14) 0.0000(11) 0.0037(12) 0.0020(12) N3 0.0178(13) 0.0196(14) 0.0201(13) -0.0010(12) 0.0011(10) 0.0023(12) N4 0.0208(15) 0.0190(14) 0.0218(13) -0.0006(11) 0.0017(11) 0.0028(12) N5 0.0195(14) 0.0172(14) 0.0246(14) -0.0017(11) 0.0020(11) -0.0011(12) N6 0.0206(14) 0.0166(14) 0.0229(14) -0.0030(11) 0.0017(11) -0.0015(12) N7 0.0274(16) 0.0224(16) 0.0303(16) -0.0013(13) 0.0004(12) 0.0045(13) N8 0.0301(16) 0.0264(17) 0.0308(16) -0.0014(13) 0.0090(13) 0.0007(14) C1 0.048(2) 0.038(2) 0.0257(18) 0.0008(17) -0.0021(17) 0.0135(19) C2 0.0261(19) 0.032(2) 0.0245(17) 0.0058(15) 0.0013(14) 0.0073(16) C3 0.037(2) 0.0260(19) 0.0286(18) 0.0074(15) 0.0040(15) 0.0099(17) C4 0.0261(19) 0.0214(18) 0.0286(18) 0.0025(14) 0.0055(14) 0.0035(15) C5 0.048(2) 0.0227(19) 0.037(2) 0.0022(16) 0.0068(18) 0.0062(18) C6 0.0208(18) 0.0263(19) 0.0322(18) -0.0010(15) 0.0023(14) -0.0034(15) C7 0.0165(17) 0.0264(19) 0.0244(17) -0.0002(14) -0.0021(13) 0.0022(15) C8 0.0165(15) 0.0275(19) 0.0234(16) 0.0036(14) 0.0015(12) -0.0001(15) C9 0.0178(16) 0.0243(18) 0.0199(15) 0.0045(13) -0.0003(12) 0.0060(14) C10 0.0249(19) 0.0292(19) 0.0234(17) -0.0006(14) 0.0026(14) 0.0050(16) C11 0.0193(18) 0.0260(19) 0.0317(18) -0.0001(15) -0.0010(14) 0.0024(15) C12 0.0188(17) 0.0235(18) 0.0210(16) 0.0022(13) 0.0020(13) -0.0033(14) C13 0.0201(18) 0.0224(18) 0.0266(17) 0.0008(14) -0.0002(13) -0.0018(15) C14 0.0247(18) 0.0224(18) 0.0227(16) -0.0001(14) 0.0012(13) -0.0023(15) C15 0.031(2) 0.0263(19) 0.036(2) -0.0068(16) -0.0029(16) 0.0005(17) C16 0.0140(16) 0.033(2) 0.0207(16) -0.0060(15) 0.0013(12) -0.0011(15) C17 0.0230(17) 0.0184(17) 0.0260(16) 0.0035(14) -0.0013(13) 0.0009(15) N9 0.0233(16) 0.0342(18) 0.0376(17) 0.0141(14) 0.0014(13) -0.0065(14) C18 0.044(3) 0.039(3) 0.129(5) 0.019(3) -0.023(3) 0.002(2) C19 0.038(2) 0.036(2) 0.052(2) 0.0170(19) -0.0098(19) -0.0109(19) C20 0.080(4) 0.044(3) 0.038(2) 0.012(2) -0.002(2) -0.014(3) C21 0.041(2) 0.032(2) 0.038(2) 0.0096(17) 0.0082(17) -0.0051(19) C22 0.042(3) 0.060(4) 0.142(6) -0.021(4) 0.025(3) 0.003(3) C23 0.033(2) 0.070(3) 0.049(3) 0.003(2) 0.0118(19) -0.015(2) C24 0.078(4) 0.070(3) 0.041(2) 0.016(2) -0.015(2) -0.038(3) C25 0.035(2) 0.042(2) 0.047(2) 0.0139(19) -0.0077(18) -0.015(2) N10 0.168(5) 0.112(4) 0.140(4) 0.018(4) 0.052(4) 0.012(4) C26 0.158(7) 0.060(4) 0.105(5) 0.016(4) 0.050(5) 0.030(5) C27 0.137(6) 0.055(4) 0.094(5) 0.011(3) 0.012(4) 0.009(4) O1 0.100(4) 0.119(4) 0.096(3) 0.023(3) 0.039(3) 0.042(3) C28 0.118(7) 0.032(5) 0.062(5) 0.013(4) 0.063(5) 0.038(5) C29 0.108(7) 0.081(6) 0.075(6) 0.020(5) 0.059(6) 0.052(6) C30 0.076(8) 0.079(6) 0.054(5) 0.010(5) 0.013(7) 0.052(7) C31 0.100(4) 0.119(4) 0.096(3) 0.023(3) 0.039(3) 0.042(3) _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 Co1 C17 1.892(3) . ? Co1 C16 1.904(4) . ? Co1 N3 1.968(3) . ? Co1 N1 1.975(3) . ? Co1 N5 2.100(3) . ? B1 N6 1.530(5) . ? B1 N2 1.542(4) . ? B1 N4 1.544(5) . ? N1 C2 1.342(4) . ? N1 N2 1.379(4) . ? N2 C4 1.358(4) . ? N3 C7 1.342(4) . ? N3 N4 1.385(4) . ? N4 C9 1.354(4) . ? N5 C12 1.331(4) . ? N5 N6 1.373(4) . ? N6 C14 1.361(4) . ? N7 C16 1.151(4) . ? N8 C17 1.156(4) . ? C1 C2 1.493(5) . ? C2 C3 1.399(5) . ? C3 C4 1.372(5) . ? C4 C5 1.493(5) . ? C6 C7 1.487(5) . ? C7 C8 1.395(4) . ? C8 C9 1.377(5) . ? C9 C10 1.499(4) . ? C11 C12 1.486(5) . ? C12 C13 1.409(4) . ? C13 C14 1.378(5) . ? C14 C15 1.489(5) . ? N9 C21 1.511(4) . ? N9 C25 1.516(5) . ? N9 C19 1.517(5) . ? N9 C23 1.523(5) . ? C18 C19 1.498(6) . ? C20 C21 1.512(6) . ? C22 C23 1.520(7) . ? C24 C25 1.529(5) . ? N10 C26 1.159(9) . ? C26 C27 1.380(8) . ? O1 C29 1.48(2) . ? O1 O1 1.539(12) 3_665 ? C28 C29 1.60(2) . ? 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 C17 Co1 C16 88.66(13) . . ? C17 Co1 N3 173.09(12) . . ? C16 Co1 N3 92.46(12) . . ? C17 Co1 N1 90.94(12) . . ? C16 Co1 N1 172.95(12) . . ? N3 Co1 N1 87.11(11) . . ? C17 Co1 N5 97.19(12) . . ? C16 Co1 N5 95.07(12) . . ? N3 Co1 N5 89.51(10) . . ? N1 Co1 N5 91.96(11) . . ? N6 B1 N2 109.0(3) . . ? N6 B1 N4 109.3(3) . . ? N2 B1 N4 106.9(3) . . ? C2 N1 N2 107.0(3) . . ? C2 N1 Co1 134.9(2) . . ? N2 N1 Co1 118.05(19) . . ? C4 N2 N1 109.3(2) . . ? C4 N2 B1 131.6(3) . . ? N1 N2 B1 118.7(3) . . ? C7 N3 N4 106.8(3) . . ? C7 N3 Co1 136.0(2) . . ? N4 N3 Co1 117.19(19) . . ? C9 N4 N3 109.5(3) . . ? C9 N4 B1 130.9(3) . . ? N3 N4 B1 119.4(3) . . ? C12 N5 N6 107.6(2) . . ? C12 N5 Co1 136.2(2) . . ? N6 N5 Co1 116.20(19) . . ? C14 N6 N5 109.6(3) . . ? C14 N6 B1 132.1(3) . . ? N5 N6 B1 118.1(2) . . ? N1 C2 C3 109.3(3) . . ? N1 C2 C1 122.4(3) . . ? C3 C2 C1 128.3(3) . . ? C4 C3 C2 106.5(3) . . ? N2 C4 C3 107.9(3) . . ? N2 C4 C5 122.6(3) . . ? C3 C4 C5 129.5(3) . . ? N3 C7 C8 109.3(3) . . ? N3 C7 C6 121.7(3) . . ? C8 C7 C6 129.0(3) . . ? C9 C8 C7 106.8(3) . . ? N4 C9 C8 107.6(3) . . ? N4 C9 C10 123.3(3) . . ? C8 C9 C10 129.1(3) . . ? N5 C12 C13 109.1(3) . . ? N5 C12 C11 122.2(3) . . ? C13 C12 C11 128.7(3) . . ? C14 C13 C12 106.4(3) . . ? N6 C14 C13 107.3(3) . . ? N6 C14 C15 122.2(3) . . ? C13 C14 C15 130.4(3) . . ? N7 C16 Co1 176.9(3) . . ? N8 C17 Co1 177.6(3) . . ? C21 N9 C25 106.2(3) . . ? C21 N9 C19 111.7(3) . . ? C25 N9 C19 111.2(3) . . ? C21 N9 C23 111.0(3) . . ? C25 N9 C23 110.8(3) . . ? C19 N9 C23 106.1(3) . . ? C18 C19 N9 114.2(3) . . ? N9 C21 C20 114.7(3) . . ? C22 C23 N9 113.8(4) . . ? N9 C25 C24 115.1(3) . . ? N10 C26 C27 179.5(10) . . ? C29 O1 O1 117.6(10) . 3_665 ? O1 C29 C28 112.5(14) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.756 _refine_diff_density_min -0.656 _refine_diff_density_rms 0.085 # Attachment '3_new.cif' # CCDC 610654 data_k05083_NEt4Tp*Ni(CN)2.CH3CN.0.5Et2O _database_code_depnum_ccdc_archive 'CCDC 610654' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H50 B N10 Ni O0.50' _chemical_formula_weight 616.31 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' 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 P2(1)/c 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 10.0820(1) _cell_length_b 13.7650(2) _cell_length_c 24.3610(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.3180(6) _cell_angle_gamma 90.00 _cell_volume 3379.89(8) _cell_formula_units_Z 4 _cell_measurement_temperature 90.0(2) _cell_measurement_reflns_used 8050 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description rod-like _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1324 _exptl_absorpt_coefficient_mu 0.610 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8382 _exptl_absorpt_correction_T_max 0.9141 _exptl_absorpt_process_details 'Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90.0(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 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\w scans at fixed \c = 55\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15099 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_sigmaI/netI 0.0869 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 27.47 _reflns_number_total 7734 _reflns_number_gt 4551 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL (Sheldrick, 1994)' _computing_publication_material ; SHELX97-2 (Sheldrick, 1997) and local procedures ; _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^)+(0.0686P)^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 7734 _refine_ls_number_parameters 438 _refine_ls_number_restraints 115 _refine_ls_R_factor_all 0.1082 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1361 _refine_ls_wR_factor_gt 0.1149 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.008 _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 Ni1 Ni 0.12537(3) 1.00540(2) 0.169728(13) 0.01833(12) Uani 1 1 d . . . B1 B 0.0987(3) 0.8356(2) 0.08620(12) 0.0205(7) Uani 1 1 d . . . H1 H 0.0777 0.7799 0.0611 0.025 Uiso 1 1 calc R . . N1 N -0.0128(2) 0.99341(14) 0.11361(8) 0.0169(5) Uani 1 1 d . . . N2 N -0.0035(2) 0.91754(15) 0.07681(8) 0.0186(5) Uani 1 1 d . . . N3 N 0.0963(2) 0.87045(16) 0.18790(9) 0.0209(5) Uani 1 1 d . . . N4 N 0.0882(2) 0.80292(16) 0.14649(9) 0.0206(5) Uani 1 1 d . . . N5 N 0.2757(2) 0.95968(16) 0.09987(9) 0.0206(5) Uani 1 1 d . . . N6 N 0.2396(2) 0.87318(16) 0.07575(8) 0.0192(5) Uani 1 1 d . . . N8 N 0.1596(2) 1.21989(17) 0.14936(10) 0.0271(6) Uani 1 1 d . . . N7 N 0.3260(2) 1.03042(17) 0.26228(10) 0.0268(6) Uani 1 1 d . . . C1 C -0.1593(3) 1.1366(2) 0.12765(11) 0.0270(7) Uani 1 1 d . . . H1A H -0.1525 1.1249 0.1673 0.040 Uiso 1 1 calc R . . H1B H -0.2513 1.1526 0.1174 0.040 Uiso 1 1 calc R . . H1C H -0.1014 1.1908 0.1180 0.040 Uiso 1 1 calc R . . C2 C -0.1179(3) 1.0472(2) 0.09758(11) 0.0200(6) Uani 1 1 d . . . C3 C -0.1756(2) 1.00681(18) 0.05031(10) 0.0187(6) Uani 1 1 d . . . H3A H -0.2509 1.0306 0.0304 0.022 Uiso 1 1 calc R . . C4 C -0.1025(3) 0.92614(19) 0.03817(10) 0.0196(6) Uani 1 1 d . . . C5 C -0.1230(3) 0.8542(2) -0.00704(10) 0.0238(6) Uani 1 1 d . . . H5A H -0.1847 0.8810 -0.0347 0.036 Uiso 1 1 calc R . . H5B H -0.1598 0.7941 0.0079 0.036 Uiso 1 1 calc R . . H5C H -0.0378 0.8402 -0.0240 0.036 Uiso 1 1 calc R . . C6 C 0.0697(3) 0.8736(2) 0.28969(11) 0.0298(7) Uani 1 1 d . . . H6A H 0.0440 0.9416 0.2841 0.045 Uiso 1 1 calc R . . H6B H 0.1577 0.8708 0.3075 0.045 Uiso 1 1 calc R . . H6C H 0.0050 0.8415 0.3130 0.045 Uiso 1 1 calc R . . C7 C 0.0735(3) 0.8229(2) 0.23542(11) 0.0230(6) Uani 1 1 d . . . C8 C 0.0492(3) 0.7251(2) 0.22356(11) 0.0255(7) Uani 1 1 d . . . H8A H 0.0298 0.6753 0.2492 0.031 Uiso 1 1 calc R . . C9 C 0.0589(3) 0.71487(19) 0.16771(11) 0.0215(6) Uani 1 1 d . . . C10 C 0.0423(3) 0.6257(2) 0.13329(12) 0.0312(7) Uani 1 1 d . . . H10A H -0.0290 0.6361 0.1059 0.047 Uiso 1 1 calc R . . H10B H 0.0196 0.5706 0.1568 0.047 Uiso 1 1 calc R . . H10C H 0.1253 0.6119 0.1146 0.047 Uiso 1 1 calc R . . C11 C 0.4660(3) 1.0705(2) 0.10163(12) 0.0282(7) Uani 1 1 d . . . H11A H 0.4443 1.0839 0.1399 0.042 Uiso 1 1 calc R . . H11B H 0.4363 1.1247 0.0784 0.042 Uiso 1 1 calc R . . H11C H 0.5622 1.0626 0.0987 0.042 Uiso 1 1 calc R . . C12 C 0.3980(3) 0.97946(19) 0.08320(11) 0.0206(6) Uani 1 1 d . . . C13 C 0.4420(3) 0.9053(2) 0.04889(11) 0.0244(6) Uani 1 1 d . . . H13A H 0.5256 0.9014 0.0318 0.029 Uiso 1 1 calc R . . C14 C 0.3400(3) 0.8392(2) 0.04484(10) 0.0215(6) Uani 1 1 d . . . C15 C 0.3293(3) 0.7465(2) 0.01319(12) 0.0317(7) Uani 1 1 d . . . H15A H 0.3147 0.6924 0.0385 0.047 Uiso 1 1 calc R . . H15B H 0.4115 0.7355 -0.0066 0.047 Uiso 1 1 calc R . . H15C H 0.2546 0.7507 -0.0132 0.047 Uiso 1 1 calc R . . C16 C 0.2468(3) 1.02114(19) 0.22724(11) 0.0215(6) Uani 1 1 d . . . C17 C 0.1441(2) 1.1376(2) 0.15768(11) 0.0203(6) Uani 1 1 d . . . N9 N 0.4161(2) 0.31225(18) 0.27943(10) 0.0327(6) Uani 1 1 d . . . C18 C 0.2712(3) 0.2981(3) 0.36326(15) 0.0600(12) Uani 1 1 d . . . H18A H 0.1971 0.2610 0.3780 0.090 Uiso 1 1 calc R . . H18B H 0.2471 0.3671 0.3613 0.090 Uiso 1 1 calc R . . H18C H 0.3496 0.2901 0.3873 0.090 Uiso 1 1 calc R . . C19 C 0.3013(3) 0.2616(2) 0.30655(13) 0.0359(8) Uani 1 1 d . . . H19A H 0.2210 0.2693 0.2828 0.043 Uiso 1 1 calc R . . H19B H 0.3213 0.1913 0.3089 0.043 Uiso 1 1 calc R . . C20 C 0.5832(3) 0.1938(3) 0.32124(15) 0.0514(10) Uani 1 1 d . . . H20A H 0.6672 0.1908 0.3422 0.077 Uiso 1 1 calc R . . H20B H 0.5937 0.1619 0.2856 0.077 Uiso 1 1 calc R . . H20C H 0.5140 0.1605 0.3417 0.077 Uiso 1 1 calc R . . C21 C 0.5441(3) 0.2985(2) 0.31235(13) 0.0350(8) Uani 1 1 d . . . H21A H 0.6165 0.3321 0.2932 0.042 Uiso 1 1 calc R . . H21B H 0.5348 0.3301 0.3486 0.042 Uiso 1 1 calc R . . C22 C 0.5471(4) 0.3004(3) 0.19078(14) 0.0601(11) Uani 1 1 d . . . H22A H 0.5428 0.2717 0.1540 0.090 Uiso 1 1 calc R . . H22B H 0.6284 0.2789 0.2099 0.090 Uiso 1 1 calc R . . H22C H 0.5472 0.3713 0.1878 0.090 Uiso 1 1 calc R . . C23 C 0.4271(3) 0.2680(2) 0.22286(13) 0.0409(9) Uani 1 1 d . . . H23A H 0.3459 0.2843 0.2012 0.049 Uiso 1 1 calc R . . H23B H 0.4302 0.1964 0.2267 0.049 Uiso 1 1 calc R . . C24 C 0.2632(4) 0.4499(3) 0.2477(2) 0.0721(13) Uani 1 1 d . . . H24A H 0.2579 0.5208 0.2456 0.108 Uiso 1 1 calc R . . H24B H 0.1887 0.4251 0.2688 0.108 Uiso 1 1 calc R . . H24C H 0.2592 0.4224 0.2106 0.108 Uiso 1 1 calc R . . C25 C 0.3929(3) 0.4207(2) 0.27597(17) 0.0520(10) Uani 1 1 d . . . H25A H 0.4670 0.4505 0.2560 0.062 Uiso 1 1 calc R . . H25B H 0.3948 0.4477 0.3137 0.062 Uiso 1 1 calc R . . N10 N 0.6842(11) 0.5327(8) -0.0946(5) 0.132(3) Uani 0.50 1 d PU A 1 C26 C 0.7828(12) 0.5650(7) -0.0793(4) 0.085(3) Uani 0.50 1 d PU A 1 C27 C 0.9103(11) 0.6041(7) -0.0599(4) 0.059(2) Uani 0.50 1 d PU A 1 H27A H 0.9761 0.5517 -0.0580 0.089 Uiso 0.50 1 calc PR A 1 H27B H 0.9005 0.6324 -0.0233 0.089 Uiso 0.50 1 calc PR A 1 H27C H 0.9399 0.6543 -0.0853 0.089 Uiso 0.50 1 calc PR A 1 N11 N 0.6823(10) 0.6391(8) 0.0435(4) 0.116(3) Uani 0.50 1 d PU B 1 C32 C 0.6628(11) 0.5652(9) 0.0640(5) 0.082(3) Uani 0.50 1 d PU B 1 C33 C 0.645(3) 0.4775(17) 0.0891(12) 0.094(5) Uani 0.50 1 d PU B 1 H33A H 0.6436 0.4869 0.1290 0.140 Uiso 0.50 1 calc PR B 1 H33B H 0.7186 0.4340 0.0801 0.140 Uiso 0.50 1 calc PR B 1 H33C H 0.5612 0.4488 0.0763 0.140 Uiso 0.50 1 calc PR B 1 C28 C 0.9885(9) 0.5991(7) -0.0473(4) 0.058(2) Uani 0.50 1 d PU C 2 H28A H 1.0053 0.6202 -0.0850 0.087 Uiso 0.50 1 calc PR C 2 H28B H 1.0317 0.5363 -0.0406 0.087 Uiso 0.50 1 calc PR C 2 H28C H 1.0243 0.6473 -0.0214 0.087 Uiso 0.50 1 calc PR C 2 C29 C 0.8330(9) 0.5884(7) -0.0393(3) 0.0545(19) Uani 0.50 1 d PU C 2 H29A H 0.7885 0.6521 -0.0439 0.065 Uiso 0.50 1 calc PR C 2 H29B H 0.7944 0.5426 -0.0666 0.065 Uiso 0.50 1 calc PR C 2 O1 O 0.8167(5) 0.5525(4) 0.0150(2) 0.0568(13) Uani 0.50 1 d PU C 2 C30 C 0.6763(9) 0.5396(7) 0.0237(4) 0.071(2) Uani 0.50 1 d PU C 2 H30A H 0.6369 0.4926 -0.0027 0.086 Uiso 0.50 1 calc PR C 2 H30B H 0.6280 0.6021 0.0206 0.086 Uiso 0.50 1 calc PR C 2 C31 C 0.675(3) 0.4982(17) 0.0855(12) 0.084(4) Uani 0.50 1 d PU C 2 H31A H 0.5832 0.4869 0.0962 0.126 Uiso 0.50 1 calc PR C 2 H31B H 0.7165 0.5456 0.1106 0.126 Uiso 0.50 1 calc PR C 2 H31C H 0.7245 0.4370 0.0874 0.126 Uiso 0.50 1 calc PR C 2 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 Ni1 0.01785(19) 0.0201(2) 0.01696(19) -0.00059(15) -0.00193(13) -0.00109(15) B1 0.0228(17) 0.0192(17) 0.0195(16) -0.0003(13) 0.0018(13) 0.0002(14) N1 0.0163(11) 0.0177(12) 0.0167(11) -0.0012(10) -0.0015(9) 0.0004(9) N2 0.0196(12) 0.0204(13) 0.0160(12) -0.0028(10) 0.0019(9) 0.0016(10) N3 0.0201(12) 0.0229(13) 0.0197(12) 0.0006(10) -0.0024(9) -0.0017(10) N4 0.0245(13) 0.0185(13) 0.0189(12) -0.0016(10) -0.0011(10) -0.0018(10) N5 0.0197(12) 0.0206(12) 0.0214(12) 0.0000(10) -0.0001(10) -0.0025(10) N6 0.0194(12) 0.0193(12) 0.0189(12) -0.0007(10) 0.0001(9) 0.0022(10) N8 0.0283(14) 0.0242(15) 0.0286(14) -0.0037(11) -0.0027(11) -0.0006(11) N7 0.0276(14) 0.0261(14) 0.0264(14) -0.0013(11) -0.0067(11) -0.0008(11) C1 0.0232(15) 0.0273(16) 0.0303(16) -0.0040(13) -0.0049(12) 0.0029(13) C2 0.0159(14) 0.0225(15) 0.0216(15) 0.0003(12) 0.0004(11) -0.0019(12) C3 0.0135(13) 0.0229(15) 0.0197(13) 0.0039(12) -0.0029(10) -0.0031(12) C4 0.0183(14) 0.0222(15) 0.0182(14) 0.0049(12) 0.0007(11) -0.0067(11) C5 0.0254(15) 0.0280(16) 0.0179(14) 0.0001(12) -0.0030(12) -0.0026(13) C6 0.0305(17) 0.0399(19) 0.0191(15) 0.0017(14) -0.0007(12) -0.0037(14) C7 0.0190(15) 0.0293(17) 0.0205(15) 0.0050(13) -0.0013(11) 0.0012(12) C8 0.0264(16) 0.0249(16) 0.0249(16) 0.0099(13) -0.0011(12) 0.0001(13) C9 0.0198(15) 0.0215(15) 0.0232(15) 0.0037(12) -0.0019(11) -0.0002(12) C10 0.0389(18) 0.0210(16) 0.0335(17) 0.0024(14) 0.0003(14) -0.0021(13) C11 0.0218(16) 0.0309(17) 0.0317(17) 0.0012(14) 0.0006(13) -0.0028(13) C12 0.0188(14) 0.0254(16) 0.0175(14) 0.0043(12) -0.0017(11) 0.0021(12) C13 0.0170(14) 0.0329(17) 0.0234(15) 0.0029(13) 0.0029(11) 0.0059(13) C14 0.0216(15) 0.0243(16) 0.0188(14) 0.0019(12) 0.0021(11) 0.0050(12) C15 0.0335(18) 0.0291(18) 0.0326(18) -0.0046(14) 0.0065(14) 0.0046(14) C16 0.0204(15) 0.0210(16) 0.0234(15) 0.0015(12) 0.0030(12) -0.0024(11) C17 0.0147(14) 0.0260(17) 0.0200(15) -0.0045(12) -0.0048(11) -0.0009(12) N9 0.0215(13) 0.0305(15) 0.0461(16) -0.0144(12) -0.0031(12) -0.0056(11) C18 0.038(2) 0.067(3) 0.076(3) -0.041(2) 0.030(2) -0.0197(19) C19 0.0188(16) 0.0336(19) 0.055(2) -0.0145(16) 0.0025(15) -0.0058(13) C20 0.029(2) 0.065(3) 0.059(2) -0.009(2) -0.0097(17) 0.0042(18) C21 0.0198(16) 0.046(2) 0.0389(19) -0.0167(16) 0.0002(14) -0.0048(14) C22 0.083(3) 0.055(3) 0.042(2) -0.0188(19) 0.012(2) -0.029(2) C23 0.044(2) 0.039(2) 0.039(2) -0.0134(16) -0.0043(16) -0.0134(16) C24 0.038(2) 0.039(2) 0.138(4) 0.011(3) -0.006(2) 0.0030(18) C25 0.035(2) 0.029(2) 0.093(3) -0.0138(19) 0.0064(19) -0.0043(15) N10 0.100(6) 0.141(6) 0.155(7) -0.042(6) -0.010(6) -0.004(5) C26 0.097(6) 0.071(6) 0.086(6) -0.026(5) -0.001(5) -0.002(5) C27 0.093(7) 0.028(4) 0.057(6) -0.006(4) 0.008(6) 0.008(6) N11 0.132(6) 0.109(6) 0.107(6) 0.008(5) 0.019(5) -0.014(5) C32 0.089(5) 0.073(6) 0.085(6) 0.003(5) 0.006(5) -0.017(5) C33 0.129(13) 0.079(9) 0.072(8) -0.003(6) -0.011(9) -0.024(9) C28 0.078(6) 0.053(5) 0.043(5) -0.007(4) 0.006(5) -0.011(6) C29 0.073(5) 0.049(4) 0.041(4) -0.010(4) -0.002(4) -0.005(4) O1 0.061(3) 0.062(3) 0.047(3) -0.006(3) 0.001(2) -0.007(3) C30 0.073(4) 0.062(5) 0.080(5) -0.005(4) 0.022(4) -0.005(4) C31 0.096(9) 0.077(10) 0.081(7) 0.003(7) 0.018(6) -0.022(7) _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 Ni1 C16 1.852(3) . ? Ni1 C17 1.854(3) . ? Ni1 N3 1.934(2) . ? Ni1 N1 1.936(2) . ? Ni1 N5 2.389(2) . ? B1 N6 1.539(4) . ? B1 N2 1.541(4) . ? B1 N4 1.542(4) . ? B1 H1 1.0000 . ? N1 C2 1.344(3) . ? N1 N2 1.381(3) . ? N2 C4 1.361(3) . ? N3 C7 1.354(3) . ? N3 N4 1.373(3) . ? N4 C9 1.353(3) . ? N5 C12 1.335(3) . ? N5 N6 1.373(3) . ? N6 C14 1.358(3) . ? N8 C17 1.162(3) . ? N7 C16 1.162(3) . ? C1 C2 1.496(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.394(3) . ? C3 C4 1.368(4) . ? C3 H3A 0.9500 . ? C4 C5 1.492(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.496(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.397(4) . ? C8 C9 1.374(4) . ? C8 H8A 0.9500 . ? C9 C10 1.494(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.493(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.398(4) . ? C13 C14 1.374(4) . ? C13 H13A 0.9500 . ? C14 C15 1.494(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? N9 C25 1.513(4) . ? N9 C23 1.513(4) . ? N9 C19 1.515(4) . ? N9 C21 1.516(4) . ? C18 C19 1.508(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.509(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.522(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.518(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? N10 C26 1.144(12) . ? C26 C27 1.462(14) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? N11 C32 1.152(13) . ? C32 C33 1.37(2) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C28 C29 1.591(12) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 O1 1.427(9) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? O1 C30 1.447(10) . ? C30 C31 1.61(3) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? 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 C16 Ni1 C17 86.38(11) . . ? C16 Ni1 N3 92.31(10) . . ? C17 Ni1 N3 174.86(10) . . ? C16 Ni1 N1 175.18(10) . . ? C17 Ni1 N1 92.65(10) . . ? N3 Ni1 N1 88.25(9) . . ? C16 Ni1 N5 98.65(10) . . ? C17 Ni1 N5 94.42(10) . . ? N3 Ni1 N5 90.69(8) . . ? N1 Ni1 N5 86.13(8) . . ? N6 B1 N2 110.3(2) . . ? N6 B1 N4 109.8(2) . . ? N2 B1 N4 107.1(2) . . ? N6 B1 H1 109.9 . . ? N2 B1 H1 109.9 . . ? N4 B1 H1 109.9 . . ? C2 N1 N2 107.0(2) . . ? C2 N1 Ni1 135.08(18) . . ? N2 N1 Ni1 117.68(15) . . ? C4 N2 N1 108.9(2) . . ? C4 N2 B1 130.0(2) . . ? N1 N2 B1 120.8(2) . . ? C7 N3 N4 107.0(2) . . ? C7 N3 Ni1 133.60(19) . . ? N4 N3 Ni1 119.28(16) . . ? C9 N4 N3 109.6(2) . . ? C9 N4 B1 130.2(2) . . ? N3 N4 B1 119.9(2) . . ? C12 N5 N6 106.5(2) . . ? C12 N5 Ni1 140.22(18) . . ? N6 N5 Ni1 111.53(15) . . ? C14 N6 N5 110.0(2) . . ? C14 N6 B1 132.7(2) . . ? N5 N6 B1 117.2(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 109.3(2) . . ? N1 C2 C1 122.6(2) . . ? C3 C2 C1 128.1(2) . . ? C4 C3 C2 106.6(2) . . ? C4 C3 H3A 126.7 . . ? C2 C3 H3A 126.7 . . ? N2 C4 C3 108.1(2) . . ? N2 C4 C5 122.6(2) . . ? C3 C4 C5 129.2(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 C8 108.7(2) . . ? N3 C7 C6 122.6(2) . . ? C8 C7 C6 128.6(3) . . ? C9 C8 C7 106.7(2) . . ? C9 C8 H8A 126.6 . . ? C7 C8 H8A 126.6 . . ? N4 C9 C8 107.9(2) . . ? N4 C9 C10 123.0(2) . . ? C8 C9 C10 129.1(2) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N5 C12 C13 109.9(2) . . ? N5 C12 C11 120.1(2) . . ? C13 C12 C11 130.0(2) . . ? C14 C13 C12 106.2(2) . . ? C14 C13 H13A 126.9 . . ? C12 C13 H13A 126.9 . . ? N6 C14 C13 107.3(2) . . ? N6 C14 C15 122.3(2) . . ? C13 C14 C15 130.4(2) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N7 C16 Ni1 178.0(3) . . ? N8 C17 Ni1 177.9(3) . . ? C25 N9 C23 111.2(3) . . ? C25 N9 C19 111.1(2) . . ? C23 N9 C19 106.5(2) . . ? C25 N9 C21 106.3(2) . . ? C23 N9 C21 110.6(2) . . ? C19 N9 C21 111.2(2) . . ? C19 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C19 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C18 C19 N9 114.7(2) . . ? C18 C19 H19A 108.6 . . ? N9 C19 H19A 108.6 . . ? C18 C19 H19B 108.6 . . ? N9 C19 H19B 108.6 . . ? H19A C19 H19B 107.6 . . ? C21 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C21 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C20 C21 N9 114.3(2) . . ? C20 C21 H21A 108.7 . . ? N9 C21 H21A 108.7 . . ? C20 C21 H21B 108.7 . . ? N9 C21 H21B 108.7 . . ? H21A C21 H21B 107.6 . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C23 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N9 C23 C22 115.2(2) . . ? N9 C23 H23A 108.5 . . ? C22 C23 H23A 108.5 . . ? N9 C23 H23B 108.5 . . ? C22 C23 H23B 108.5 . . ? H23A C23 H23B 107.5 . . ? C25 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C25 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N9 C25 C24 114.6(3) . . ? N9 C25 H25A 108.6 . . ? C24 C25 H25A 108.6 . . ? N9 C25 H25B 108.6 . . ? C24 C25 H25B 108.6 . . ? H25A C25 H25B 107.6 . . ? N10 C26 C27 178.7(12) . . ? N11 C32 C33 177.5(18) . . ? C29 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C29 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O1 C29 C28 106.3(6) . . ? O1 C29 H29A 110.5 . . ? C28 C29 H29A 110.5 . . ? O1 C29 H29B 110.5 . . ? C28 C29 H29B 110.5 . . ? H29A C29 H29B 108.7 . . ? C29 O1 C30 108.2(6) . . ? O1 C30 C31 102.1(11) . . ? O1 C30 H30A 111.3 . . ? C31 C30 H30A 111.3 . . ? O1 C30 H30B 111.3 . . ? C31 C30 H30B 111.3 . . ? H30A C30 H30B 109.2 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.023 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.076