# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_1 _database_code_CSD 179190 _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Datta, Dipankar' 'Chowdhury, Shubhamoy' 'Drew, Michael G. B.' 'Pal, P. K.' _publ_contact_author_name 'Dr Dipankar Datta' _publ_contact_author_address ; Department of Inorganic Chemistry Indian Association for the Cultivation of Science Calcutta 700 032 INDIA ; _publ_contact_author_email 'ICDD@MAHENDRA.IACS.RES.IN' _publ_section_title ; The electrooxidation of the tetraphenylborate ion revisited ; _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H50 B Cu N6 O' _chemical_formula_weight 885.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.779(17) _cell_length_b 13.887(17) _cell_length_c 16.42(2) _cell_angle_alpha 87.558(10) _cell_angle_beta 80.704(10) _cell_angle_gamma 83.014(10) _cell_volume 2408(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 0.498 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.221 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 4 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7997 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0756 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 26.16 _reflns_number_total 7997 _reflns_number_gt 4112 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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^)+(0.1574P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7997 _refine_ls_number_parameters 581 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1656 _refine_ls_R_factor_gt 0.0758 _refine_ls_wR_factor_ref 0.2431 _refine_ls_wR_factor_gt 0.2032 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _refine_ls_shift/su_max 0.073 _refine_ls_shift/su_mean 0.004 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 Cu1 Cu 0.69629(6) 0.51839(5) 0.69900(3) 0.0747(3) Uani 1 d . . . N1 N 0.7103(4) 0.5505(3) 0.8123(2) 0.0711(11) Uani 1 d . . . C2 C 0.7273(5) 0.6353(5) 0.8403(3) 0.0860(16) Uani 1 d . . . H2 H 0.7352 0.6871 0.8028 0.103 Uiso 1 calc R . . C3 C 0.7339(7) 0.6517(6) 0.9212(4) 0.108(2) Uani 1 d . . . H3 H 0.7475 0.7124 0.9375 0.130 Uiso 1 calc R . . C4 C 0.7202(7) 0.5778(7) 0.9766(4) 0.110(2) Uani 1 d . . . H4 H 0.7235 0.5878 1.0318 0.132 Uiso 1 calc R . . C5 C 0.7016(6) 0.4880(6) 0.9525(3) 0.0922(18) Uani 1 d . . . H5 H 0.6913 0.4370 0.9906 0.111 Uiso 1 calc R . . C6 C 0.6984(4) 0.4755(4) 0.8677(3) 0.0692(14) Uani 1 d . . . C7 C 0.6863(4) 0.3794(4) 0.8346(3) 0.0661(13) Uani 1 d . . . N8 N 0.6905(3) 0.3809(3) 0.7560(2) 0.0636(10) Uani 1 d . . . N9 N 0.6722(3) 0.3001(3) 0.7165(2) 0.0635(10) Uani 1 d . . . C10 C 0.7629(4) 0.2630(3) 0.6610(3) 0.0575(11) Uani 1 d . . . C11 C 0.8931(4) 0.2956(3) 0.6429(2) 0.0538(11) Uani 1 d . . . N12 N 0.9162(3) 0.3798(3) 0.6119(2) 0.0593(9) Uani 1 d . . . N13 N 0.8149(3) 0.4477(3) 0.6018(2) 0.0603(10) Uani 1 d . . . C14 C 0.7891(4) 0.4709(3) 0.5295(3) 0.0584(11) Uani 1 d . . . C200 C 0.8607(5) 0.4280(4) 0.4522(3) 0.0873(17) Uani 1 d . . . H20A H 0.9267 0.3798 0.4651 0.105 Uiso 1 calc R . . H20B H 0.8973 0.4780 0.4175 0.105 Uiso 1 calc R . . H20C H 0.8044 0.3985 0.4237 0.105 Uiso 1 calc R . . C15 C 0.6778(4) 0.5457(3) 0.5292(3) 0.0567(11) Uani 1 d . . . C16 C 0.6319(5) 0.5782(4) 0.4570(3) 0.0757(14) Uani 1 d . . . H16 H 0.6731 0.5549 0.4063 0.091 Uiso 1 calc R . . C17 C 0.5266(5) 0.6443(4) 0.4608(4) 0.0819(15) Uani 1 d . . . H17 H 0.4956 0.6661 0.4129 0.098 Uiso 1 calc R . . C18 C 0.4664(5) 0.6787(4) 0.5368(4) 0.0845(16) Uani 1 d . . . H18 H 0.3952 0.7244 0.5410 0.101 Uiso 1 calc R . . C19 C 0.5152(5) 0.6430(4) 0.6060(3) 0.0800(15) Uani 1 d . . . H19 H 0.4748 0.6656 0.6572 0.096 Uiso 1 calc R . . N20 N 0.6189(4) 0.5767(3) 0.6037(2) 0.0661(10) Uani 1 d . . . C100 C 0.6720(7) 0.2915(5) 0.8889(4) 0.105(2) Uani 1 d . . . H10A H 0.6928 0.2345 0.8561 0.126 Uiso 1 calc R . . H10B H 0.5861 0.2939 0.9165 0.126 Uiso 1 calc R . . H10C H 0.7278 0.2894 0.9291 0.126 Uiso 1 calc R . . C30 C 0.7365(4) 0.1829(3) 0.6115(3) 0.0560(11) Uani 1 d . . . C31 C 0.8168(5) 0.1512(4) 0.5412(3) 0.0691(13) Uani 1 d . . . H31 H 0.8910 0.1795 0.5248 0.083 Uiso 1 calc R . . C32 C 0.7898(6) 0.0788(4) 0.4950(3) 0.0805(15) Uani 1 d . . . H32 H 0.8448 0.0586 0.4477 0.097 Uiso 1 calc R . . C33 C 0.6812(6) 0.0365(4) 0.5192(4) 0.0890(18) Uani 1 d . . . H33 H 0.6629 -0.0132 0.4886 0.107 Uiso 1 calc R . . C34 C 0.5988(5) 0.0674(4) 0.5889(4) 0.0821(16) Uani 1 d . . . H34 H 0.5239 0.0397 0.6041 0.099 Uiso 1 calc R . . C35 C 0.6268(4) 0.1378(4) 0.6350(3) 0.0687(13) Uani 1 d . . . H35 H 0.5723 0.1564 0.6831 0.082 Uiso 1 calc R . . C40 C 1.0029(4) 0.2246(3) 0.6569(3) 0.0557(11) Uani 1 d . . . C41 C 1.1273(4) 0.2437(4) 0.6238(4) 0.0772(15) Uani 1 d . . . H41 H 1.1404 0.2991 0.5913 0.093 Uiso 1 calc R . . C42 C 1.2281(5) 0.1801(5) 0.6401(4) 0.099(2) Uani 1 d . . . H42 H 1.3099 0.1938 0.6198 0.119 Uiso 1 calc R . . C43 C 1.2107(5) 0.0961(4) 0.6859(4) 0.0932(18) Uani 1 d . . . H43 H 1.2804 0.0532 0.6953 0.112 Uiso 1 calc R . . C44 C 1.0906(5) 0.0755(4) 0.7179(3) 0.0778(14) Uani 1 d . . . H44 H 1.0788 0.0189 0.7490 0.093 Uiso 1 calc R . . C45 C 0.9867(4) 0.1405(4) 0.7033(3) 0.0645(12) Uani 1 d . . . H45 H 0.9054 0.1269 0.7251 0.077 Uiso 1 calc R . . B1 B 1.1384(5) 0.7319(4) 0.8255(3) 0.0622(14) Uani 1 d . . . C61 C 1.2667(4) 0.7867(3) 0.7990(3) 0.0617(12) Uani 1 d . . . C62 C 1.2999(4) 0.8270(3) 0.7202(3) 0.0635(12) Uani 1 d . . . H62 H 1.2430 0.8285 0.6831 0.076 Uiso 1 calc R . . C63 C 1.4128(5) 0.8644(4) 0.6949(4) 0.0798(15) Uani 1 d . . . H63 H 1.4312 0.8888 0.6412 0.096 Uiso 1 calc R . . C64 C 1.4981(5) 0.8662(5) 0.7481(4) 0.0918(18) Uani 1 d . . . H64 H 1.5736 0.8926 0.7313 0.110 Uiso 1 calc R . . C65 C 1.4704(5) 0.8285(5) 0.8265(4) 0.101(2) Uani 1 d . . . H65 H 1.5276 0.8291 0.8632 0.121 Uiso 1 calc R . . C66 C 1.3568(5) 0.7892(5) 0.8513(3) 0.0841(16) Uani 1 d . . . H66 H 1.3402 0.7636 0.9047 0.101 Uiso 1 calc R . . C71 C 1.0890(4) 0.7376(4) 0.9253(3) 0.0650(13) Uani 1 d . . . C72 C 1.0425(5) 0.6595(5) 0.9730(3) 0.0802(15) Uani 1 d . . . H72 H 1.0454 0.6005 0.9476 0.096 Uiso 1 calc R . . C73 C 0.9927(6) 0.6662(6) 1.0557(4) 0.101(2) Uani 1 d . . . H73 H 0.9618 0.6124 1.0840 0.121 Uiso 1 calc R . . C74 C 0.9879(7) 0.7490(7) 1.0962(4) 0.111(2) Uani 1 d . . . H74 H 0.9551 0.7524 1.1521 0.134 Uiso 1 calc R . . C75 C 1.0333(6) 0.8305(6) 1.0529(4) 0.1013(19) Uani 1 d . . . H75 H 1.0305 0.8888 1.0793 0.122 Uiso 1 calc R . . C76 C 1.0825(5) 0.8214(5) 0.9695(3) 0.0844(16) Uani 1 d . . . H76 H 1.1132 0.8754 0.9414 0.101 Uiso 1 calc R . . C81 C 1.1775(4) 0.6176(4) 0.7999(2) 0.0609(12) Uani 1 d . . . C82 C 1.2993(5) 0.5696(4) 0.8000(3) 0.0756(14) Uani 1 d . . . H82 H 1.3616 0.6043 0.8132 0.091 Uiso 1 calc R . . C83 C 1.3312(6) 0.4722(5) 0.7810(4) 0.0896(18) Uani 1 d . . . H83 H 1.4140 0.4439 0.7806 0.108 Uiso 1 calc R . . C85 C 1.2421(8) 0.4175(5) 0.7628(3) 0.0944(19) Uani 1 d . . . H85 H 1.2631 0.3520 0.7516 0.113 Uiso 1 calc R . . C84 C 1.1204(7) 0.4617(5) 0.7616(3) 0.0888(18) Uani 1 d . . . H84 H 1.0591 0.4259 0.7485 0.107 Uiso 1 calc R . . C86 C 1.0891(5) 0.5597(4) 0.7798(3) 0.0723(14) Uani 1 d . . . H86 H 1.0065 0.5877 0.7786 0.087 Uiso 1 calc R . . C92 C 1.0207(5) 0.7683(5) 0.6949(3) 0.0863(17) Uani 1 d . . . H92 H 1.0822 0.7225 0.6680 0.104 Uiso 1 calc R . . C93 C 0.9318(6) 0.8144(6) 0.6501(4) 0.111(2) Uani 1 d . . . H93 H 0.9324 0.7979 0.5958 0.134 Uiso 1 calc R . . C94 C 0.8435(6) 0.8840(6) 0.6866(5) 0.112(2) Uani 1 d . . . H94 H 0.7856 0.9181 0.6566 0.134 Uiso 1 calc R . . C96 C 0.9299(5) 0.8559(4) 0.8111(3) 0.0776(15) Uani 1 d . . . H96 H 0.9266 0.8718 0.8660 0.093 Uiso 1 calc R . . C95 C 0.8403(5) 0.9035(5) 0.7667(5) 0.105(2) Uani 1 d . . . H95 H 0.7775 0.9492 0.7924 0.126 Uiso 1 calc R . . C91 C 1.0249(4) 0.7851(4) 0.7763(3) 0.0617(12) Uani 1 d . . . C101 C 0.6297(13) 0.9015(13) 1.0589(13) 0.212(7) Uani 1 d . . . O102 O 0.5704(13) 0.8559(10) 1.0238(9) 0.303(6) Uani 1 d . . . C103 C 0.7014(18) 0.9683(13) 1.0147(13) 0.328(13) Uani 1 d . . . H10D H 0.7263 1.0107 1.0522 0.393 Uiso 1 calc R . . H10E H 0.6521 1.0057 0.9782 0.393 Uiso 1 calc R . . H10F H 0.7755 0.9347 0.9830 0.393 Uiso 1 calc R . . C104 C 0.6290(18) 0.8827(17) 1.1407(11) 0.335(14) Uani 1 d . . . H10G H 0.7012 0.9060 1.1573 0.402 Uiso 1 calc R . . H10H H 0.6323 0.8140 1.1513 0.402 Uiso 1 calc R . . H10I H 0.5529 0.9148 1.1714 0.402 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0825(5) 0.0786(5) 0.0608(4) -0.0032(3) -0.0118(3) 0.0012(3) N1 0.062(3) 0.078(3) 0.072(3) -0.009(2) -0.0106(18) 0.000(2) C2 0.094(4) 0.081(4) 0.081(4) -0.024(3) -0.014(3) 0.002(3) C3 0.127(6) 0.107(5) 0.094(5) -0.027(4) -0.021(4) -0.017(4) C4 0.125(6) 0.142(7) 0.068(4) -0.034(4) -0.017(3) -0.021(5) C5 0.091(4) 0.119(5) 0.068(3) -0.007(3) -0.014(3) -0.013(4) C6 0.051(3) 0.095(4) 0.061(3) -0.010(3) -0.009(2) -0.001(2) C7 0.051(3) 0.084(4) 0.062(3) 0.008(3) -0.0071(19) -0.007(2) N8 0.058(2) 0.070(3) 0.062(2) -0.008(2) -0.0051(16) -0.0095(19) N9 0.054(2) 0.073(3) 0.062(2) 0.003(2) -0.0010(17) -0.0102(19) C10 0.046(3) 0.064(3) 0.063(3) 0.004(2) -0.0105(19) -0.011(2) C11 0.039(2) 0.070(3) 0.053(2) -0.009(2) -0.0065(16) -0.009(2) N12 0.051(2) 0.058(3) 0.069(2) -0.0015(19) -0.0093(16) -0.0110(18) N13 0.053(2) 0.059(2) 0.067(2) -0.0014(18) -0.0045(16) -0.0076(17) C14 0.057(3) 0.062(3) 0.056(3) -0.001(2) -0.0009(19) -0.018(2) C200 0.093(4) 0.101(4) 0.060(3) -0.006(3) 0.001(2) 0.003(3) C15 0.055(3) 0.057(3) 0.061(3) 0.005(2) -0.0111(19) -0.018(2) C16 0.087(4) 0.081(4) 0.064(3) 0.005(3) -0.020(2) -0.023(3) C17 0.084(4) 0.077(4) 0.090(4) 0.019(3) -0.034(3) -0.009(3) C18 0.084(4) 0.073(4) 0.097(4) 0.010(3) -0.025(3) 0.000(3) C19 0.073(3) 0.080(4) 0.081(3) 0.007(3) -0.007(2) 0.005(3) N20 0.068(3) 0.065(3) 0.063(2) 0.0011(18) -0.0074(17) -0.004(2) C100 0.129(5) 0.116(5) 0.076(4) 0.013(4) -0.015(3) -0.044(4) C30 0.048(3) 0.054(3) 0.070(3) 0.005(2) -0.018(2) -0.014(2) C31 0.061(3) 0.076(4) 0.076(3) -0.009(3) -0.017(2) -0.018(3) C32 0.092(4) 0.084(4) 0.075(3) -0.016(3) -0.025(3) -0.025(3) C33 0.105(5) 0.064(4) 0.117(5) -0.004(3) -0.059(4) -0.030(3) C34 0.070(4) 0.076(4) 0.110(4) 0.008(4) -0.028(3) -0.030(3) C35 0.057(3) 0.064(3) 0.087(3) 0.007(3) -0.012(2) -0.016(2) C40 0.050(3) 0.058(3) 0.063(3) -0.014(2) -0.0123(18) -0.010(2) C41 0.046(3) 0.064(3) 0.121(4) -0.012(3) -0.007(2) -0.011(2) C42 0.043(3) 0.084(4) 0.169(6) -0.013(4) -0.011(3) -0.011(3) C43 0.056(4) 0.075(4) 0.151(6) -0.015(4) -0.027(3) 0.000(3) C44 0.081(4) 0.067(3) 0.088(3) 0.001(3) -0.024(3) -0.006(3) C45 0.051(3) 0.070(3) 0.075(3) -0.001(2) -0.017(2) -0.008(2) B1 0.049(3) 0.072(4) 0.066(3) 0.002(3) -0.010(2) -0.010(3) C61 0.048(3) 0.063(3) 0.073(3) -0.005(2) -0.007(2) -0.003(2) C62 0.056(3) 0.056(3) 0.078(3) 0.004(2) -0.006(2) -0.015(2) C63 0.066(3) 0.077(4) 0.092(4) 0.006(3) 0.002(3) -0.014(3) C64 0.061(4) 0.099(5) 0.117(5) 0.004(4) 0.000(3) -0.037(3) C65 0.061(4) 0.132(6) 0.119(5) -0.020(4) -0.034(3) -0.019(4) C66 0.057(3) 0.111(5) 0.087(4) 0.007(3) -0.018(2) -0.017(3) C71 0.056(3) 0.086(4) 0.056(2) -0.003(3) -0.0083(19) -0.014(2) C72 0.074(3) 0.102(4) 0.065(3) -0.003(3) -0.002(2) -0.022(3) C73 0.102(5) 0.133(6) 0.072(4) -0.006(4) 0.002(3) -0.047(4) C74 0.115(5) 0.153(7) 0.069(4) -0.019(4) 0.008(3) -0.049(5) C75 0.095(4) 0.115(5) 0.094(4) -0.036(4) -0.007(3) -0.014(4) C76 0.075(4) 0.106(5) 0.070(3) -0.012(3) -0.002(2) -0.014(3) C81 0.058(3) 0.078(3) 0.045(2) 0.003(2) 0.0015(18) -0.017(2) C82 0.065(3) 0.073(4) 0.085(3) 0.001(3) -0.003(2) -0.011(3) C83 0.079(4) 0.091(5) 0.091(4) 0.007(3) 0.001(3) -0.001(4) C85 0.131(6) 0.077(4) 0.065(3) 0.004(3) 0.008(3) -0.006(4) C84 0.122(5) 0.081(4) 0.067(3) 0.004(3) -0.001(3) -0.049(4) C86 0.061(3) 0.082(4) 0.074(3) -0.006(3) -0.002(2) -0.021(3) C92 0.061(3) 0.131(5) 0.065(3) 0.003(3) -0.010(2) -0.004(3) C93 0.063(4) 0.194(8) 0.075(4) 0.023(4) -0.009(3) -0.012(4) C94 0.061(4) 0.153(7) 0.116(5) 0.046(5) -0.017(3) -0.007(4) C96 0.058(3) 0.085(4) 0.088(3) 0.002(3) -0.006(2) -0.010(3) C95 0.057(4) 0.123(5) 0.123(5) 0.023(4) -0.003(3) 0.005(3) C91 0.047(3) 0.073(3) 0.064(3) 0.009(2) -0.0021(19) -0.018(2) C101 0.145(10) 0.246(17) 0.272(18) -0.120(15) -0.076(11) -0.030(10) O102 0.294(14) 0.327(16) 0.337(15) -0.023(12) -0.127(12) -0.118(12) C103 0.232(18) 0.221(17) 0.49(3) -0.089(18) 0.118(19) -0.061(14) C104 0.32(3) 0.50(4) 0.193(15) -0.010(18) -0.098(15) 0.01(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 Cu1 N1 1.965(5) . ? Cu1 N20 1.987(4) . ? Cu1 N13 2.077(4) . ? Cu1 N8 2.094(5) . ? N1 C2 1.327(7) . ? N1 C6 1.358(6) . ? C2 C3 1.372(8) . ? C3 C4 1.347(9) . ? C4 C5 1.371(10) . ? C5 C6 1.418(7) . ? C6 C7 1.489(8) . ? C7 N8 1.285(6) . ? C7 C100 1.490(7) . ? N8 N9 1.370(6) . ? N9 C10 1.297(6) . ? C10 C30 1.487(7) . ? C10 C11 1.506(6) . ? C11 N12 1.292(6) . ? C11 C40 1.488(6) . ? N12 N13 1.379(5) . ? N13 C14 1.283(5) . ? C14 C200 1.483(6) . ? C14 C15 1.488(6) . ? C15 N20 1.347(6) . ? C15 C16 1.394(6) . ? C16 C17 1.365(8) . ? C17 C18 1.386(8) . ? C18 C19 1.377(7) . ? C19 N20 1.355(6) . ? C30 C31 1.379(7) . ? C30 C35 1.398(7) . ? C31 C32 1.371(7) . ? C32 C33 1.366(8) . ? C33 C34 1.379(9) . ? C34 C35 1.352(8) . ? C40 C45 1.380(6) . ? C40 C41 1.415(7) . ? C41 C42 1.369(7) . ? C42 C43 1.376(8) . ? C43 C44 1.375(8) . ? C44 C45 1.396(6) . ? B1 C71 1.641(7) . ? B1 C61 1.647(7) . ? B1 C81 1.647(8) . ? B1 C91 1.657(6) . ? C61 C62 1.397(6) . ? C61 C66 1.402(7) . ? C62 C63 1.377(7) . ? C63 C64 1.370(8) . ? C64 C65 1.370(8) . ? C65 C66 1.395(8) . ? C71 C76 1.386(8) . ? C71 C72 1.405(7) . ? C72 C73 1.381(7) . ? C73 C74 1.345(9) . ? C74 C75 1.406(9) . ? C75 C76 1.392(8) . ? C81 C82 1.398(7) . ? C81 C86 1.406(7) . ? C82 C83 1.390(8) . ? C83 C85 1.371(9) . ? C85 C84 1.382(9) . ? C84 C86 1.395(8) . ? C92 C91 1.376(7) . ? C92 C93 1.380(7) . ? C93 C94 1.357(10) . ? C94 C95 1.348(9) . ? C96 C95 1.391(8) . ? C96 C91 1.399(7) . ? C101 O102 1.180(13) . ? C101 C104 1.357(19) . ? C101 C103 1.38(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 N1 Cu1 N20 139.31(18) . . ? N1 Cu1 N13 135.78(17) . . ? N20 Cu1 N13 79.35(17) . . ? N1 Cu1 N8 80.02(19) . . ? N20 Cu1 N8 130.88(17) . . ? N13 Cu1 N8 85.88(16) . . ? C2 N1 C6 117.4(5) . . ? C2 N1 Cu1 128.2(4) . . ? C6 N1 Cu1 114.4(4) . . ? N1 C2 C3 124.2(6) . . ? C4 C3 C2 118.5(7) . . ? C3 C4 C5 120.8(6) . . ? C4 C5 C6 117.9(6) . . ? N1 C6 C5 121.2(6) . . ? N1 C6 C7 116.8(4) . . ? C5 C6 C7 121.9(5) . . ? N8 C7 C6 113.3(4) . . ? N8 C7 C100 124.5(5) . . ? C6 C7 C100 122.2(5) . . ? C7 N8 N9 120.6(4) . . ? C7 N8 Cu1 115.0(4) . . ? N9 N8 Cu1 123.6(3) . . ? C10 N9 N8 118.1(4) . . ? N9 C10 C30 117.7(4) . . ? N9 C10 C11 124.7(4) . . ? C30 C10 C11 117.6(4) . . ? N12 C11 C40 117.7(4) . . ? N12 C11 C10 124.2(4) . . ? C40 C11 C10 118.1(4) . . ? C11 N12 N13 118.2(3) . . ? C14 N13 N12 120.4(4) . . ? C14 N13 Cu1 115.8(3) . . ? N12 N13 Cu1 123.7(3) . . ? N13 C14 C200 124.4(4) . . ? N13 C14 C15 113.8(4) . . ? C200 C14 C15 121.8(4) . . ? N20 C15 C16 121.4(5) . . ? N20 C15 C14 116.0(4) . . ? C16 C15 C14 122.6(4) . . ? C17 C16 C15 120.0(5) . . ? C16 C17 C18 119.4(5) . . ? C19 C18 C17 117.9(5) . . ? N20 C19 C18 123.6(5) . . ? C15 N20 C19 117.7(4) . . ? C15 N20 Cu1 115.0(3) . . ? C19 N20 Cu1 127.3(3) . . ? C31 C30 C35 117.8(5) . . ? C31 C30 C10 122.1(4) . . ? C35 C30 C10 120.1(4) . . ? C32 C31 C30 121.5(5) . . ? C33 C32 C31 119.4(6) . . ? C32 C33 C34 120.3(6) . . ? C35 C34 C33 120.1(5) . . ? C34 C35 C30 120.8(5) . . ? C45 C40 C41 118.7(4) . . ? C45 C40 C11 121.4(4) . . ? C41 C40 C11 119.9(4) . . ? C42 C41 C40 119.5(5) . . ? C41 C42 C43 121.2(5) . . ? C44 C43 C42 120.2(5) . . ? C43 C44 C45 119.4(5) . . ? C40 C45 C44 120.9(4) . . ? C71 B1 C61 111.1(4) . . ? C71 B1 C81 109.4(4) . . ? C61 B1 C81 106.6(4) . . ? C71 B1 C91 108.9(4) . . ? C61 B1 C91 109.3(4) . . ? C81 B1 C91 111.6(4) . . ? C62 C61 C66 114.5(4) . . ? C62 C61 B1 122.8(4) . . ? C66 C61 B1 122.5(4) . . ? C63 C62 C61 123.2(5) . . ? C64 C63 C62 120.5(5) . . ? C65 C64 C63 119.0(5) . . ? C64 C65 C66 120.2(5) . . ? C65 C66 C61 122.6(5) . . ? C76 C71 C72 113.7(5) . . ? C76 C71 B1 123.2(5) . . ? C72 C71 B1 123.0(5) . . ? C73 C72 C71 123.1(6) . . ? C74 C73 C72 121.2(6) . . ? C73 C74 C75 119.1(6) . . ? C76 C75 C74 118.2(6) . . ? C71 C76 C75 124.6(6) . . ? C82 C81 C86 114.9(5) . . ? C82 C81 B1 122.8(5) . . ? C86 C81 B1 122.3(4) . . ? C83 C82 C81 122.8(6) . . ? C85 C83 C82 120.8(6) . . ? C83 C85 C84 118.7(6) . . ? C85 C84 C86 120.3(6) . . ? C84 C86 C81 122.5(5) . . ? C91 C92 C93 124.8(5) . . ? C94 C93 C92 119.1(6) . . ? C95 C94 C93 119.6(5) . . ? C95 C96 C91 122.3(6) . . ? C94 C95 C96 120.6(6) . . ? C92 C91 C96 113.6(4) . . ? C92 C91 B1 122.7(4) . . ? C96 C91 B1 123.6(4) . . ? O102 C101 C104 118(2) . . ? O102 C101 C103 119(2) . . ? C104 C101 C103 122.9(16) . . ? _refine_diff_density_max 0.343 _refine_diff_density_min -0.704 _refine_diff_density_rms 0.067 #===END