Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_coden_Cambridge 0186 loop_ _publ_author_name 'Mark D. Spicer' 'Mark Garner' 'Krzysztof Lewinski' 'Agnieszka Pattek-Janczyk' 'John Reglinski' ; B.Sieklucka ; 'Maciej Szaleniec' _publ_contact_author_name 'Dr Mark D. Spicer ' _publ_contact_author_address ; Pure & applied Chemistry University of strathclyde 295 Cathedral Street GLASGOW G1 1XL UNITED KINGDOM ; _publ_contact_author_email M.D.SPICER@STRATH.AC.UK _publ_section_title ; Structural and spectroscopic characterisation of iron(II), nickel(II) and nickel(III) complexes of the hydrotris(methimazolyl)borate anion: soft donors in a weak ligand field ; data_nitm2br _database_code_CSD 195022 _audit_creation_date 2002-11-21T10:11:55-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common [Ni(Tm)2]Br.4(CH2Cl2) _chemical_formula_moiety 'C24 H32 B2 Br1 N12 Ni1 S6, 4(C H2 CL2)' _chemical_formula_sum 'C28 H40 B2 Br1 Cl8 N12 Ni1 S6' _chemical_formula_weight 1180.92 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting cubic _symmetry_space_group_name_H-M P213 _symmetry_space_group_name_Hall 'P 2ac 2ab 3' _symmetry_Int_Tables_number 198 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' 'y, z, x' '-y+1/2, -z, x+1/2' 'y+1/2, -z+1/2, -x' '-y, z+1/2, -x+1/2' 'z, x, y' '-z, x+1/2, -y+1/2' '-z+1/2, -x, y+1/2' 'z+1/2, -x+1/2, -y' _cell_length_a 16.8111(4) _cell_length_b 16.8111(4) _cell_length_c 16.8111(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4751.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 1778 _cell_measurement_theta_min 1.455 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2372 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.002 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_UB_11 0.0141452 _diffrn_orient_matrix_UB_12 0.0302774 _diffrn_orient_matrix_UB_13 0.0492097 _diffrn_orient_matrix_UB_21 -0.0153822 _diffrn_orient_matrix_UB_22 -0.0468612 _diffrn_orient_matrix_UB_23 0.0332539 _diffrn_orient_matrix_UB_31 0.055693 _diffrn_orient_matrix_UB_32 -0.0206329 _diffrn_orient_matrix_UB_33 -0.003314 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_unetI/netI 0.0207 _diffrn_reflns_number 1771 _diffrn_reflns_limit_h_min 2 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 26.26 _diffrn_reflns_theta_full 26.26 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 1771 _reflns_number_gt 1660 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0342P)^2^+31.5216P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 1771 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0668 _refine_ls_wR_factor_ref 0.1608 _refine_ls_wR_factor_gt 0.1588 _refine_ls_goodness_of_fit_ref 1.185 _refine_ls_restrained_S_all 1.185 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.48(4) _refine_diff_density_max 0.512 _refine_diff_density_min -0.783 _refine_diff_density_rms 0.105 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Br Br -0.2901 2.4595 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _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 C1 C 0.2157(7) 0.0334(6) 0.1312(7) 0.042(2) Uani 1 1 d . . . C2 C 0.1191(8) -0.0600(7) 0.1339(8) 0.050(3) Uani 1 1 d . . . H2 H 0.0699 -0.0866 0.1257 0.061 Uiso 1 1 calc R . . C3 C 0.1828(8) -0.0899(7) 0.1707(7) 0.047(3) Uani 1 1 d . . . H3 H 0.187 -0.1408 0.1948 0.056 Uiso 1 1 calc R . . C4 C 0.3223(8) -0.0439(7) 0.1985(9) 0.056(3) Uani 1 1 d . . . H4A H 0.3613 -0.0218 0.1613 0.085 Uiso 1 1 calc R . . H4B H 0.3323 -0.101 0.2054 0.085 Uiso 1 1 calc R . . H4C H 0.3272 -0.017 0.25 0.085 Uiso 1 1 calc R . . C5 C 0.3836(6) 0.3019(6) 0.2033(7) 0.042(2) Uani 1 1 d . . . C6 C 0.5118(7) 0.2767(7) 0.2230(8) 0.050(3) Uani 1 1 d . . . H6 H 0.5654 0.2609 0.2143 0.06 Uiso 1 1 calc R . . C7 C 0.4822(6) 0.3039(7) 0.2898(8) 0.046(3) Uani 1 1 d . . . H7 H 0.5111 0.3114 0.3377 0.055 Uiso 1 1 calc R . . C8 C 0.4570(8) 0.2488(9) 0.0843(7) 0.060(4) Uani 1 1 d . . . H8A H 0.5074 0.2207 0.0759 0.09 Uiso 1 1 calc R . . H8B H 0.4546 0.2952 0.0491 0.09 Uiso 1 1 calc R . . H8C H 0.4126 0.2131 0.0724 0.09 Uiso 1 1 calc R . . C9 C 0.5828(7) 0.2203(8) 0.4809(9) 0.053(3) Uani 1 1 d . . . H9A H 0.615 0.2013 0.5264 0.064 Uiso 1 1 calc R . . H9B H 0.6126 0.209 0.4314 0.064 Uiso 1 1 calc R . . C10 C 0.440(3) 0.083(3) 0.888(3) 0.063(12) Uani 0.33 1 d P . . B1 B 0.0714(9) 0.0714(9) 0.0714(9) 0.045(5) Uani 1 3 d S . . H1 H 0.0371 0.0371 0.0371 0.054 Uiso 1 3 calc SR . . B2 B 0.3484(8) 0.3484(8) 0.3484(8) 0.047(5) Uani 1 3 d S . . H2A H 0.3828 0.3828 0.3828 0.057 Uiso 1 3 calc SR . . N1 N 0.1374(6) 0.0172(5) 0.1095(6) 0.041(2) Uani 1 1 d . . . N2 N 0.2418(6) -0.0320(6) 0.1669(6) 0.048(2) Uani 1 1 d . . . N3 N 0.4518(6) 0.2751(6) 0.1678(6) 0.049(2) Uani 1 1 d . . . N4 N 0.4004(5) 0.3202(5) 0.2790(6) 0.041(2) Uani 1 1 d . . . Cl1 Cl 0.5672(2) 0.3238(2) 0.4897(2) 0.0683(10) Uani 1 1 d . . . Cl2 Cl 0.4901(2) 0.1689(2) 0.4791(2) 0.0678(10) Uani 1 1 d . . . Cl3 Cl 0.4701(3) 0.0299(3) 0.9701(3) 0.105(3) Uani 1 3 d S . . Cl4 Cl 0.3414(7) 0.1176(8) 0.9069(7) 0.075(3) Uani 0.33 1 d P . . Br1 Br 0.71281(6) 0.21281(6) 0.28719(6) 0.0409(4) Uani 1 3 d S . . Ni1 Ni 0.21017(8) 0.21017(8) 0.21017(8) 0.0366(5) Uani 1 3 d S . . S1 S 0.26651(18) 0.11968(19) 0.11730(18) 0.0456(7) Uani 1 1 d . . . S2 S 0.29386(17) 0.30910(16) 0.15453(16) 0.0407(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.047(6) 0.035(5) 0.045(6) -0.009(5) 0.001(5) -0.003(5) C2 0.053(7) 0.040(6) 0.059(8) -0.012(6) -0.011(6) -0.005(6) C3 0.063(8) 0.032(5) 0.046(6) 0.006(5) -0.003(6) 0.007(5) C4 0.061(8) 0.044(7) 0.064(8) -0.004(6) -0.024(7) 0.006(6) C5 0.041(5) 0.038(6) 0.045(6) 0.009(5) 0.007(5) 0.001(5) C6 0.041(6) 0.050(7) 0.060(8) 0.013(6) -0.003(6) -0.003(5) C7 0.029(5) 0.059(7) 0.050(7) 0.011(6) -0.001(5) 0.002(5) C8 0.052(7) 0.086(10) 0.042(7) 0.008(7) 0.003(6) -0.002(7) C9 0.045(7) 0.049(7) 0.065(8) -0.002(7) 0.000(6) -0.001(6) C10 0.07(3) 0.05(2) 0.07(3) 0.01(3) 0.02(2) 0.03(2) B1 0.045(5) 0.045(5) 0.045(5) 0.000(6) 0.000(6) 0.000(6) B2 0.047(5) 0.047(5) 0.047(5) -0.006(6) -0.006(6) -0.006(6) N1 0.040(5) 0.036(5) 0.047(5) -0.003(4) -0.002(4) 0.000(4) N2 0.062(6) 0.036(5) 0.045(5) -0.007(4) -0.006(5) -0.003(5) N3 0.038(5) 0.056(6) 0.053(6) 0.004(5) 0.012(5) -0.003(5) N4 0.036(5) 0.038(5) 0.050(5) 0.005(4) -0.002(4) 0.000(4) Cl1 0.079(2) 0.069(2) 0.058(2) -0.0046(18) -0.0080(18) -0.0049(19) Cl2 0.0555(19) 0.072(2) 0.076(2) 0.009(2) 0.0015(18) -0.0082(17) Cl3 0.105(3) 0.105(3) 0.105(3) 0.016(3) -0.016(3) 0.016(3) Cl4 0.069(7) 0.085(8) 0.070(7) 0.000(7) 0.015(6) 0.009(7) Br1 0.0409(4) 0.0409(4) 0.0409(4) 0.0015(5) 0.0015(5) -0.0015(5) Ni1 0.0366(5) 0.0366(5) 0.0366(5) -0.0024(6) -0.0024(6) -0.0024(6) S1 0.0470(16) 0.0485(16) 0.0412(15) 0.0026(13) -0.0080(13) -0.0086(13) S2 0.0391(14) 0.0420(15) 0.0411(14) 0.0063(11) -0.0014(12) -0.0013(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 N2 1.327(14) . ? C1 N1 1.394(15) . ? C1 S1 1.699(11) . ? C2 C3 1.334(17) . ? C2 N1 1.395(15) . ? C3 N2 1.391(15) . ? C4 N2 1.469(15) . ? C5 N4 1.340(15) . ? C5 N3 1.369(14) . ? C5 S2 1.721(11) . ? C6 C7 1.310(17) . ? C6 N3 1.371(15) . ? C7 N4 1.413(13) . ? C8 N3 1.474(16) . ? C9 Cl1 1.765(13) . ? C9 Cl2 1.782(12) . ? C10 C10 1.09(7) 6_565 ? C10 C10 1.09(7) 12_456 ? C10 Cl4 1.26(5) 6_565 ? C10 Cl4 1.40(4) 12_456 ? C10 Cl3 1.72(4) . ? C10 Cl4 1.79(4) . ? B1 N1 1.572(12) 5 ? B1 N1 1.572(12) 9 ? B1 N1 1.572(12) . ? B2 N4 1.533(12) . ? B2 N4 1.533(12) 9 ? B2 N4 1.533(12) 5 ? Cl3 C10 1.72(4) 6_565 ? Cl3 C10 1.72(4) 12_456 ? Cl4 C10 1.26(5) 12_456 ? Cl4 Cl4 1.363(19) 12_456 ? Cl4 Cl4 1.363(19) 6_565 ? Cl4 C10 1.40(4) 6_565 ? Ni1 S2 2.371(3) 9 ? Ni1 S2 2.371(3) 5 ? Ni1 S2 2.371(3) . ? Ni1 S1 2.377(3) . ? Ni1 S1 2.377(3) 9 ? Ni1 S1 2.377(3) 5 ? 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 N2 C1 N1 105.5(10) . . ? N2 C1 S1 127.1(10) . . ? N1 C1 S1 127.3(9) . . ? C3 C2 N1 108.0(11) . . ? C2 C3 N2 106.7(10) . . ? N4 C5 N3 108.2(10) . . ? N4 C5 S2 128.5(8) . . ? N3 C5 S2 123.4(9) . . ? C7 C6 N3 107.9(11) . . ? C6 C7 N4 109.1(11) . . ? Cl1 C9 Cl2 110.5(7) . . ? C10 C10 C10 60.000(18) 6_565 12_456 ? C10 C10 Cl4 99(2) 6_565 6_565 ? C10 C10 Cl4 72(4) 12_456 6_565 ? C10 C10 Cl4 59(3) 6_565 12_456 ? C10 C10 Cl4 92(3) 12_456 12_456 ? Cl4 C10 Cl4 62(2) 6_565 12_456 ? C10 C10 Cl3 71.5(11) 6_565 . ? C10 C10 Cl3 71.5(11) 12_456 . ? Cl4 C10 Cl3 142(4) 6_565 . ? Cl4 C10 Cl3 130(3) 12_456 . ? C10 C10 Cl4 51(2) 6_565 . ? C10 C10 Cl4 43.8(18) 12_456 . ? Cl4 C10 Cl4 49.3(16) 6_565 . ? Cl4 C10 Cl4 48.6(13) 12_456 . ? Cl3 C10 Cl4 107(2) . . ? N1 B1 N1 111.0(9) 5 9 ? N1 B1 N1 111.0(9) 5 . ? N1 B1 N1 111.0(9) 9 . ? N4 B2 N4 112.0(8) . 9 ? N4 B2 N4 112.0(8) . 5 ? N4 B2 N4 112.0(8) 9 5 ? C1 N1 C2 108.3(10) . . ? C1 N1 B1 131.2(11) . . ? C2 N1 B1 120.3(11) . . ? C1 N2 C3 111.4(10) . . ? C1 N2 C4 125.5(11) . . ? C3 N2 C4 123.1(10) . . ? C5 N3 C6 108.4(10) . . ? C5 N3 C8 124.3(11) . . ? C6 N3 C8 127.3(11) . . ? C5 N4 C7 106.4(10) . . ? C5 N4 B2 132.3(11) . . ? C7 N4 B2 121.2(11) . . ? C10 Cl3 C10 37(2) . 6_565 ? C10 Cl3 C10 37(2) . 12_456 ? C10 Cl3 C10 37(2) 6_565 12_456 ? C10 Cl4 Cl4 86.3(18) 12_456 12_456 ? C10 Cl4 Cl4 64(3) 12_456 6_565 ? Cl4 Cl4 Cl4 60.000(2) 12_456 6_565 ? C10 Cl4 C10 48(3) 12_456 6_565 ? Cl4 Cl4 C10 54(3) 12_456 6_565 ? Cl4 Cl4 C10 81(2) 6_565 6_565 ? C10 Cl4 C10 37(2) 12_456 . ? Cl4 Cl4 C10 50.2(18) 12_456 . ? Cl4 Cl4 C10 44.4(17) 6_565 . ? C10 Cl4 C10 37(2) 6_565 . ? S2 Ni1 S2 95.43(11) 9 5 ? S2 Ni1 S2 95.43(11) 9 . ? S2 Ni1 S2 95.43(11) 5 . ? S2 Ni1 S1 176.29(10) 9 . ? S2 Ni1 S1 81.82(10) 5 . ? S2 Ni1 S1 87.33(10) . . ? S2 Ni1 S1 87.33(10) 9 9 ? S2 Ni1 S1 176.29(10) 5 9 ? S2 Ni1 S1 81.82(10) . 9 ? S1 Ni1 S1 95.53(11) . 9 ? S2 Ni1 S1 81.82(10) 9 5 ? S2 Ni1 S1 87.33(10) 5 5 ? S2 Ni1 S1 176.29(10) . 5 ? S1 Ni1 S1 95.53(11) . 5 ? S1 Ni1 S1 95.53(11) 9 5 ? C1 S1 Ni1 104.8(4) . . ? C5 S2 Ni1 106.4(4) . . ? #end data_Fe(Tm)2 _database_code_CSD 195023 _audit_creation_date 2003-01-21T10:10:14-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[Fe(Tm)2]. 4.5H2O' _chemical_formula_moiety 'C24 H32 B2 Fe1 N12 S6' _chemical_formula_sum 'C24 H41 B2 Fe1 N12 O4.5 S6' _chemical_formula_weight 839.52 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3 _symmetry_Int_Tables_number 148 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 14.8890(6) _cell_length_b 14.8890(6) _cell_length_c 15.5697(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 2989.1(2) _cell_formula_units_Z 3 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 1353 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour Black _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.741 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_UB_11 -0.0727233 _diffrn_orient_matrix_UB_12 -0.0238426 _diffrn_orient_matrix_UB_13 0.0125488 _diffrn_orient_matrix_UB_21 -0.0320741 _diffrn_orient_matrix_UB_22 0.0085868 _diffrn_orient_matrix_UB_23 0.0700866 _diffrn_orient_matrix_UB_31 -0.0219335 _diffrn_orient_matrix_UB_32 0.0578848 _diffrn_orient_matrix_UB_33 -0.0171294 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_unetI/netI 0.0312 _diffrn_reflns_number 3074 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 1361 _reflns_number_gt 1152 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0912P)^2^+23.6903P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 1361 _refine_ls_number_parameters 81 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.177 _refine_ls_wR_factor_gt 0.1696 _refine_ls_goodness_of_fit_ref 1.09 _refine_ls_restrained_S_all 1.09 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.013 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.113 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' S S 0.1246 0.1234 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O1 O 0.4939(10) 0.2328(10) 0.8055(7) 0.109(5) Uani 0.5 1 d P . . O2 O 0.3333 0.1667 0.6667 0.143(10) Uani 0.5 2 d SP . . H1 H 0 0 0.6727 0.04(2) Uiso 1 3 d S . . Fe1 Fe 0 0 1 0.0239(4) Uani 1 6 d S . . S1 S 0.16057(7) 0.10004(7) 0.91721(6) 0.0270(3) Uani 1 1 d . . . B1 B 0 0 0.7377(5) 0.0281(16) Uani 1 3 d S . . N2 N 0.0916(3) -0.0147(3) 0.7666(2) 0.0276(7) Uani 1 1 d . . . C1 C 0.1567(3) 0.0208(3) 0.8344(2) 0.0272(8) Uani 1 1 d . . . N1 N 0.2227(3) -0.0157(3) 0.8282(2) 0.0324(8) Uani 1 1 d . . . C3 C 0.1184(3) -0.0755(3) 0.7178(3) 0.0330(9) Uani 1 1 d . . . H3 H 0.0851 -0.1106 0.6663 0.04 Uiso 1 1 calc R . . C2 C 0.1991(3) -0.0767(4) 0.7551(3) 0.0363(10) Uani 1 1 d . . . H2 H 0.2332 -0.1123 0.7354 0.044 Uiso 1 1 calc R . . C4 C 0.3061(4) 0.0055(4) 0.8873(3) 0.0428(11) Uiso 1 1 d . . . H4A H 0.3513 0.0806 0.8933 0.064 Uiso 1 1 calc R . . H4B H 0.3465 -0.025 0.8651 0.064 Uiso 1 1 calc R . . H4C H 0.277 -0.0248 0.9434 0.064 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 O1 0.131(9) 0.148(11) 0.079(7) 0.085(7) 0.089(7) 0.095(9) O2 0.23(2) 0.023(5) 0.141(14) 0.026(7) 0.148(15) 0.041(9) Fe1 0.0246(5) 0.0246(5) 0.0224(7) 0 0 0.0123(2) S1 0.0263(5) 0.0266(5) 0.0255(6) -0.0013(4) 0.0009(4) 0.0113(4) B1 0.032(2) 0.032(2) 0.020(3) 0 0 0.0160(12) N2 0.0280(16) 0.0299(17) 0.0254(16) -0.0008(13) 0.0023(13) 0.0149(14) C1 0.0272(19) 0.028(2) 0.0246(18) 0.0009(15) 0.0031(15) 0.0129(16) N1 0.0290(17) 0.039(2) 0.0327(17) -0.0027(15) -0.0001(14) 0.0193(16) C3 0.038(2) 0.036(2) 0.027(2) -0.0059(16) 0.0002(17) 0.0198(19) C2 0.039(2) 0.041(2) 0.035(2) -0.0063(18) 0.0016(18) 0.024(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Fe1 S1 2.4566(9) 12_557 ? Fe1 S1 2.4566(9) 3 ? Fe1 S1 2.4566(9) . ? Fe1 S1 2.4566(9) 2 ? Fe1 S1 2.4566(9) 10_557 ? Fe1 S1 2.4566(9) 11_557 ? S1 C1 1.728(4) . ? B1 N2 1.552(4) 2 ? B1 N2 1.552(4) . ? B1 N2 1.552(4) 3 ? N2 C1 1.350(5) . ? N2 C3 1.384(5) . ? C1 N1 1.345(5) . ? N1 C2 1.386(5) . ? N1 C4 1.448(6) . ? C3 C2 1.344(6) . ? 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 S1 Fe1 S1 180.0000(10) 12_557 3 ? S1 Fe1 S1 85.01(3) 12_557 . ? S1 Fe1 S1 94.99(3) 3 . ? S1 Fe1 S1 85.01(3) 12_557 2 ? S1 Fe1 S1 94.99(3) 3 2 ? S1 Fe1 S1 94.99(3) . 2 ? S1 Fe1 S1 94.99(3) 12_557 10_557 ? S1 Fe1 S1 85.01(3) 3 10_557 ? S1 Fe1 S1 180.00(4) . 10_557 ? S1 Fe1 S1 85.01(3) 2 10_557 ? S1 Fe1 S1 94.99(3) 12_557 11_557 ? S1 Fe1 S1 85.01(3) 3 11_557 ? S1 Fe1 S1 85.01(3) . 11_557 ? S1 Fe1 S1 180 2 11_557 ? S1 Fe1 S1 94.99(3) 10_557 11_557 ? C1 S1 Fe1 106.69(13) . . ? N2 B1 N2 112.0(3) 2 . ? N2 B1 N2 112.0(3) 2 3 ? N2 B1 N2 112.0(3) . 3 ? C1 N2 C3 107.6(3) . . ? C1 N2 B1 132.9(4) . . ? C3 N2 B1 119.6(4) . . ? N2 C1 N1 108.1(3) . . ? N2 C1 S1 128.6(3) . . ? N1 C1 S1 123.3(3) . . ? C1 N1 C2 109.1(3) . . ? C1 N1 C4 125.9(4) . . ? C2 N1 C4 125.0(4) . . ? C2 C3 N2 108.8(4) . . ? C3 C2 N1 106.4(4) . . ? #end data_nitm _database_code_CSD 195024 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C24 H32 B2 N12 Ni S6' _chemical_formula_sum 'C24 H32 B2 N12 Ni S6' _chemical_formula_weight 761.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni Ni 0.3393 1.1124 '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' S S 0.1246 0.1234 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.1690(3) _cell_length_b 9.8790(3) _cell_length_c 16.8980(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.2180(12) _cell_angle_gamma 90.00 _cell_volume 1680.13(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 527 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 23.53 _exptl_crystal_description plate _exptl_crystal_colour 'light brown' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 0.989 _exptl_absorpt_correction_type None _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans with the \k offsets' _diffrn_reflns_number 6498 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0716 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3852 _reflns_number_gt 2611 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius BV, 1997-2000)' _computing_cell_refinement 'DENZO-SMN (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 ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0273P)^2^+0.5831P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0036(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3852 _refine_ls_number_parameters 270 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0815 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.0919 _refine_ls_wR_factor_gt 0.0793 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.5000 0.5000 0.5000 0.02686(15) Uani 1 d S . . B B 0.3348(3) 0.6259(4) 0.6928(2) 0.0323(8) Uani 1 d . . . H1 H 0.291(3) 0.661(3) 0.7477(17) 0.027(7) Uiso 1 d . . . S1 S 0.39618(7) 0.33990(7) 0.58600(5) 0.03342(19) Uani 1 d . . . C11 C 0.2510(3) 0.4144(3) 0.60378(17) 0.0315(7) Uani 1 d . . . N12 N 0.2342(2) 0.5268(2) 0.64674(14) 0.0310(6) Uani 1 d . . . C13 C 0.0988(3) 0.5523(4) 0.6410(2) 0.0406(8) Uani 1 d . . . H13 H 0.070(3) 0.621(3) 0.669(2) 0.049(11) Uiso 1 d . . . C14 C 0.0333(3) 0.4561(4) 0.5968(2) 0.0439(8) Uani 1 d . . . H14 H -0.056(3) 0.448(3) 0.5777(19) 0.046(9) Uiso 1 d . . . N15 N 0.1278(2) 0.3689(3) 0.57372(16) 0.0379(6) Uani 1 d . . . C16 C 0.0992(5) 0.2492(5) 0.5252(3) 0.0580(11) Uani 1 d . . . H161 H 0.015(5) 0.243(4) 0.503(3) 0.080(14) Uiso 1 d . . . H162 H 0.117(5) 0.165(5) 0.554(3) 0.100(17) Uiso 1 d . . . H163 H 0.156(5) 0.241(6) 0.482(3) 0.13(2) Uiso 1 d . . . S2 S 0.62946(7) 0.62345(8) 0.61232(4) 0.03226(19) Uani 1 d . . . C21 C 0.5844(3) 0.5459(3) 0.69497(17) 0.0306(7) Uani 1 d . . . N22 N 0.4676(2) 0.5553(3) 0.72481(14) 0.0321(6) Uani 1 d . . . C23 C 0.4748(3) 0.4694(4) 0.79049(19) 0.0438(8) Uani 1 d . . . H23 H 0.402(3) 0.460(3) 0.818(2) 0.050(10) Uiso 1 d . . . C24 C 0.5940(3) 0.4104(4) 0.8017(2) 0.0479(9) Uani 1 d . . . H24 H 0.637(3) 0.341(3) 0.835(2) 0.054(10) Uiso 1 d . . . N25 N 0.6627(2) 0.4587(3) 0.74301(15) 0.0403(7) Uani 1 d . . . C26 C 0.7972(4) 0.4206(6) 0.7328(3) 0.0639(13) Uani 1 d . . . H261 H 0.846(5) 0.505(5) 0.739(3) 0.093(17) Uiso 1 d . . . H262 H 0.835(5) 0.377(5) 0.776(3) 0.096(17) Uiso 1 d . . . H263 H 0.793(7) 0.357(7) 0.687(4) 0.18(3) Uiso 1 d . . . S3 S 0.31126(7) 0.65504(8) 0.48613(4) 0.03283(19) Uani 1 d . . . C31 C 0.3356(3) 0.7712(3) 0.56147(18) 0.0303(6) Uani 1 d . . . N32 N 0.3492(2) 0.7533(2) 0.64165(15) 0.0315(6) Uani 1 d . . . C33 C 0.3682(3) 0.8803(3) 0.6775(2) 0.0405(8) Uani 1 d . . . H33 H 0.383(3) 0.886(3) 0.734(2) 0.047(10) Uiso 1 d . . . C34 C 0.3656(4) 0.9740(3) 0.6214(2) 0.0470(9) Uani 1 d . . . H34 H 0.371(3) 1.068(4) 0.625(2) 0.049(10) Uiso 1 d . . . N35 N 0.3455(3) 0.9067(3) 0.54829(16) 0.0392(6) Uani 1 d . . . C36 C 0.3317(5) 0.9686(5) 0.4698(3) 0.0595(11) Uani 1 d . . . H361 H 0.382(5) 0.920(6) 0.435(3) 0.11(2) Uiso 1 d . . . H362 H 0.359(4) 1.055(5) 0.475(2) 0.074(14) Uiso 1 d . . . H363 H 0.237(5) 0.964(5) 0.443(3) 0.096(16) Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.0281(3) 0.0257(3) 0.0270(3) -0.0014(2) 0.0048(2) -0.0003(2) B 0.0282(17) 0.0386(19) 0.0305(18) -0.0007(16) 0.0055(15) 0.0046(15) S1 0.0341(4) 0.0273(4) 0.0397(4) 0.0017(3) 0.0081(3) -0.0002(3) C11 0.0306(15) 0.0368(16) 0.0270(15) 0.0092(13) 0.0040(12) -0.0025(13) N12 0.0263(12) 0.0368(14) 0.0309(13) 0.0041(11) 0.0079(10) 0.0019(10) C13 0.0291(16) 0.056(2) 0.0379(19) 0.0080(17) 0.0097(14) 0.0086(16) C14 0.0248(15) 0.064(2) 0.0425(19) 0.0082(18) 0.0029(14) -0.0034(16) N15 0.0290(13) 0.0458(15) 0.0386(15) 0.0028(13) 0.0038(11) -0.0090(12) C16 0.051(2) 0.052(2) 0.067(3) -0.013(2) -0.006(2) -0.017(2) S2 0.0317(4) 0.0367(4) 0.0286(4) -0.0016(3) 0.0051(3) -0.0071(3) C21 0.0290(14) 0.0380(16) 0.0230(15) -0.0014(13) -0.0028(12) -0.0042(13) N22 0.0290(12) 0.0412(14) 0.0262(13) 0.0032(11) 0.0045(10) -0.0025(11) C23 0.0379(18) 0.063(2) 0.0310(18) 0.0101(16) 0.0074(15) -0.0030(17) C24 0.0393(18) 0.065(2) 0.038(2) 0.0186(18) -0.0005(15) 0.0037(18) N25 0.0298(13) 0.0542(17) 0.0356(15) 0.0098(13) 0.0003(11) 0.0024(12) C26 0.035(2) 0.095(4) 0.061(3) 0.024(3) 0.0047(19) 0.021(2) S3 0.0332(4) 0.0346(4) 0.0299(4) -0.0022(3) 0.0019(3) 0.0031(3) C31 0.0250(14) 0.0296(15) 0.0360(17) -0.0002(13) 0.0032(12) 0.0032(12) N32 0.0303(13) 0.0329(13) 0.0320(13) -0.0063(11) 0.0065(11) 0.0011(11) C33 0.0400(18) 0.0361(18) 0.046(2) -0.0108(17) 0.0077(16) 0.0013(14) C34 0.050(2) 0.0285(18) 0.064(2) -0.0097(17) 0.0126(18) -0.0007(15) N35 0.0455(15) 0.0275(13) 0.0450(16) 0.0023(12) 0.0073(13) -0.0003(12) C36 0.076(3) 0.045(2) 0.057(3) 0.015(2) 0.007(2) -0.001(2) _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 S3 2.4404(7) 3_666 ? Ni S3 2.4404(7) . ? Ni S2 2.4715(7) . ? Ni S2 2.4715(7) 3_666 ? Ni S1 2.4834(8) 3_666 ? Ni S1 2.4834(8) . ? B N12 1.543(4) . ? B N32 1.546(4) . ? B N22 1.547(4) . ? B H1 1.14(3) . ? S1 C11 1.714(3) . ? C11 N12 1.351(4) . ? C11 N15 1.360(4) . ? N12 C13 1.390(4) . ? C13 C14 1.328(5) . ? C13 H13 0.91(3) . ? C14 N15 1.387(4) . ? C14 H14 0.93(3) . ? N15 C16 1.445(5) . ? C16 H161 0.88(4) . ? C16 H162 0.97(5) . ? C16 H163 0.99(6) . ? S2 C21 1.712(3) . ? C21 N22 1.359(4) . ? C21 N25 1.360(4) . ? N22 C23 1.391(4) . ? C23 C24 1.333(5) . ? C23 H23 0.93(3) . ? C24 N25 1.377(4) . ? C24 H24 0.95(3) . ? N25 C26 1.452(5) . ? C26 H261 0.97(5) . ? C26 H262 0.88(5) . ? C26 H263 0.99(7) . ? S3 C31 1.706(3) . ? C31 N32 1.354(4) . ? C31 N35 1.363(4) . ? N32 C33 1.394(4) . ? C33 C34 1.322(5) . ? C33 H33 0.94(3) . ? C34 N35 1.392(4) . ? N35 C36 1.449(5) . ? C36 H361 0.95(6) . ? C36 H362 0.90(4) . ? C36 H363 1.01(5) . ? 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 S3 Ni S3 180.0 3_666 . ? S3 Ni S2 84.87(2) 3_666 . ? S3 Ni S2 95.13(2) . . ? S3 Ni S2 95.13(2) 3_666 3_666 ? S3 Ni S2 84.87(2) . 3_666 ? S2 Ni S2 180.0 . 3_666 ? S3 Ni S1 93.53(2) 3_666 3_666 ? S3 Ni S1 86.47(2) . 3_666 ? S2 Ni S1 84.88(2) . 3_666 ? S2 Ni S1 95.12(2) 3_666 3_666 ? S3 Ni S1 86.47(2) 3_666 . ? S3 Ni S1 93.53(2) . . ? S2 Ni S1 95.12(2) . . ? S2 Ni S1 84.88(2) 3_666 . ? S1 Ni S1 180.0 3_666 . ? N12 B N32 110.0(2) . . ? N12 B N22 111.9(3) . . ? N32 B N22 114.5(2) . . ? N12 B H1 107.1(14) . . ? N32 B H1 106.7(14) . . ? N22 B H1 106.0(13) . . ? C11 S1 Ni 106.14(10) . . ? N12 C11 N15 107.0(3) . . ? N12 C11 S1 128.7(2) . . ? N15 C11 S1 124.3(2) . . ? C11 N12 C13 108.2(3) . . ? C11 N12 B 131.8(2) . . ? C13 N12 B 119.9(3) . . ? C14 C13 N12 108.8(3) . . ? C14 C13 H13 131(2) . . ? N12 C13 H13 120(2) . . ? C13 C14 N15 106.9(3) . . ? C13 C14 H14 131(2) . . ? N15 C14 H14 122(2) . . ? C11 N15 C14 109.2(3) . . ? C11 N15 C16 125.6(3) . . ? C14 N15 C16 125.2(3) . . ? N15 C16 H161 113(3) . . ? N15 C16 H162 114(3) . . ? H161 C16 H162 104(4) . . ? N15 C16 H163 113(3) . . ? H161 C16 H163 108(4) . . ? H162 C16 H163 103(4) . . ? C21 S2 Ni 103.32(10) . . ? N22 C21 N25 106.9(3) . . ? N22 C21 S2 128.5(2) . . ? N25 C21 S2 124.7(2) . . ? C21 N22 C23 107.7(3) . . ? C21 N22 B 131.9(3) . . ? C23 N22 B 119.9(3) . . ? C24 C23 N22 108.8(3) . . ? C24 C23 H23 131(2) . . ? N22 C23 H23 120(2) . . ? C23 C24 N25 106.9(3) . . ? C23 C24 H24 137(2) . . ? N25 C24 H24 116(2) . . ? C21 N25 C24 109.6(3) . . ? C21 N25 C26 125.0(3) . . ? C24 N25 C26 125.4(3) . . ? N25 C26 H261 104(3) . . ? N25 C26 H262 110(3) . . ? H261 C26 H262 100(4) . . ? N25 C26 H263 109(4) . . ? H261 C26 H263 127(5) . . ? H262 C26 H263 107(5) . . ? C31 S3 Ni 108.81(10) . . ? N32 C31 N35 107.0(3) . . ? N32 C31 S3 129.9(2) . . ? N35 C31 S3 123.0(2) . . ? C31 N32 C33 107.7(3) . . ? C31 N32 B 131.5(3) . . ? C33 N32 B 120.5(3) . . ? C34 C33 N32 109.3(3) . . ? C34 C33 H33 132(2) . . ? N32 C33 H33 119(2) . . ? C33 C34 N35 106.7(3) . . ? C31 N35 C34 109.2(3) . . ? C31 N35 C36 124.3(3) . . ? C34 N35 C36 126.5(3) . . ? N35 C36 H361 111(3) . . ? N35 C36 H362 109(3) . . ? H361 C36 H362 111(4) . . ? N35 C36 H363 111(3) . . ? H361 C36 H363 105(4) . . ? H362 C36 H363 111(4) . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 0.319 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.073