# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email gxjin@fudan.edu.cn _publ_contact_author_name 'Guo-Xin Jin' _publ_author_name 'Guo-Xin Jin' data_mo_10401a _database_code_depnum_ccdc_archive 'CCDC 873635' #TrackingRef '- 3_rev_Compound-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H32 B20 Cu2 O11' _chemical_formula_weight 683.65 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' O O 0.0106 0.0060 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.3006(17) _cell_length_b 12.7704(9) _cell_length_c 13.8440(10) _cell_angle_alpha 90.00 _cell_angle_beta 123.0280(10) _cell_angle_gamma 90.00 _cell_volume 3601.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5363 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 27.89 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 1.221 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7184 _exptl_absorpt_correction_T_max 0.9194 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.80 _diffrn_reflns_number 13410 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.91 _reflns_number_total 4286 _reflns_number_gt 3586 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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. In this data, 8 DFIX and 2 ISOR instructions were used to refine one MeOH molecule coordinated with Cu1 so that there were 20 restraints. ; _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^)+(0.0519P)^2^+1.3575P] 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 4286 _refine_ls_number_parameters 237 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0846 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 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 Cu1 Cu 0.303423(10) 0.305489(15) 0.570365(17) 0.01461(8) Uani 1 1 d D . . O1 O 0.25370(7) 0.41481(11) 0.45571(12) 0.0299(3) Uani 1 1 d . . . O2 O 0.16324(7) 0.32277(10) 0.33679(12) 0.0276(3) Uani 1 1 d . . . O3 O 0.25534(7) 0.66015(12) 0.14318(12) 0.0280(3) Uani 1 1 d . . . O4 O 0.16474(7) 0.75222(12) 0.02338(12) 0.0286(3) Uani 1 1 d . . . O5 O 0.38333(7) 0.40781(11) 0.67928(13) 0.0321(3) Uani 1 1 d D . . H5' H 0.4091(13) 0.391(2) 0.7449(16) 0.048 Uiso 1 1 d D . . B3 B 0.21680(11) 0.59385(16) 0.29922(17) 0.0199(4) Uani 1 1 d . . . H3 H 0.2714 0.5861 0.3459 0.024 Uiso 1 1 calc R . . B4 B 0.17772(13) 0.61715(17) 0.3732(2) 0.0276(5) Uani 1 1 d . . . H4 H 0.2065 0.6242 0.4694 0.033 Uiso 1 1 calc R . . B5 B 0.09932(12) 0.55446(18) 0.2948(2) 0.0275(5) Uani 1 1 d . . . H5 H 0.0768 0.5201 0.3400 0.033 Uiso 1 1 calc R . . B6 B 0.08972(11) 0.49317(17) 0.17101(19) 0.0244(4) Uani 1 1 d . . . H6 H 0.0609 0.4191 0.1345 0.029 Uiso 1 1 calc R . . B7 B 0.16227(10) 0.51675(15) 0.17352(17) 0.0186(4) Uani 1 1 d . . . H7 H 0.1813 0.4587 0.1379 0.022 Uiso 1 1 calc R . . B8 B 0.17870(13) 0.71591(17) 0.2844(2) 0.0270(5) Uani 1 1 d . . . H8 H 0.2080 0.7897 0.3200 0.032 Uiso 1 1 calc R . . B9 B 0.10561(15) 0.69176(18) 0.2825(2) 0.0345(6) Uani 1 1 d . . . H9 H 0.0866 0.7495 0.3185 0.041 Uiso 1 1 calc R . . B10 B 0.05149(12) 0.61545(19) 0.1580(2) 0.0330(5) Uani 1 1 d . . . H10 H -0.0031 0.6228 0.1120 0.040 Uiso 1 1 calc R . . B11 B 0.09080(11) 0.59279(18) 0.08276(19) 0.0251(4) Uani 1 1 d . . . H11 H 0.0628 0.5862 -0.0134 0.030 Uiso 1 1 calc R . . B12 B 0.10037(12) 0.71476(18) 0.1511(2) 0.0283(5) Uani 1 1 d . . . H12 H 0.0784 0.7880 0.0995 0.034 Uiso 1 1 calc R . . C1 C 0.16526(9) 0.50279(13) 0.29831(15) 0.0176(3) Uani 1 1 d . . . C2 C 0.16686(9) 0.64983(14) 0.16724(15) 0.0178(3) Uani 1 1 d . . . C3 C 0.19684(9) 0.40413(13) 0.36969(15) 0.0184(3) Uani 1 1 d . . . C4 C 0.19879(9) 0.69165(13) 0.10608(15) 0.0180(3) Uani 1 1 d . . . C5 C 0.3736(3) 0.5169(4) 0.6814(5) 0.0571(13) Uani 0.70 1 d PU A 1 H5A H 0.4161 0.5513 0.7317 0.086 Uiso 0.70 1 calc PR A 1 H5B H 0.3455 0.5297 0.7106 0.086 Uiso 0.70 1 calc PR A 1 H5C H 0.3526 0.5453 0.6032 0.086 Uiso 0.70 1 calc PR A 1 C5' C 0.3840(7) 0.5136(9) 0.6442(11) 0.053(3) Uani 0.30 1 d PDU A 2 H5'1 H 0.3489 0.5537 0.6415 0.080 Uiso 0.30 1 calc PR A 2 H5'2 H 0.3773 0.5131 0.5676 0.080 Uiso 0.30 1 calc PR A 2 H5'3 H 0.4265 0.5460 0.6995 0.080 Uiso 0.30 1 calc PR A 2 C6 C 0.0000 0.2740(3) 0.2500 0.0517(10) Uani 1 2 d SD . . H6A H 0.0419(12) 0.313(2) 0.276(3) 0.078 Uiso 1 1 d D . . H6B H 0.005(3) 0.252(5) 0.325(3) 0.078 Uiso 0.50 1 d PD . . O6 O 0.00527(18) 0.1700(4) 0.3001(3) 0.0534(10) Uani 0.50 1 d PD . . H6' H 0.0450(14) 0.152(3) 0.329(5) 0.080 Uiso 0.50 1 d PD . . 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 0.01597(12) 0.01306(12) 0.01609(12) -0.00032(8) 0.00957(9) 0.00075(8) O1 0.0278(8) 0.0202(7) 0.0275(7) 0.0080(6) 0.0059(6) 0.0001(6) O2 0.0256(7) 0.0183(6) 0.0296(7) 0.0073(5) 0.0090(6) 0.0004(5) O3 0.0252(7) 0.0356(8) 0.0308(7) 0.0139(6) 0.0202(6) 0.0068(6) O4 0.0284(7) 0.0349(8) 0.0299(7) 0.0159(6) 0.0206(6) 0.0082(6) O5 0.0238(8) 0.0211(7) 0.0372(8) -0.0064(6) 0.0074(7) -0.0029(6) B3 0.0221(10) 0.0194(9) 0.0184(9) 0.0026(7) 0.0112(8) -0.0016(8) B4 0.0460(14) 0.0197(10) 0.0275(11) 0.0015(8) 0.0269(11) 0.0033(10) B5 0.0319(12) 0.0256(11) 0.0390(12) 0.0130(9) 0.0283(11) 0.0101(9) B6 0.0178(10) 0.0260(11) 0.0285(11) 0.0085(8) 0.0121(9) 0.0007(8) B7 0.0213(10) 0.0174(9) 0.0191(9) 0.0021(7) 0.0122(8) -0.0010(8) B8 0.0431(14) 0.0176(10) 0.0284(11) 0.0008(8) 0.0247(11) 0.0015(9) B9 0.0546(17) 0.0243(11) 0.0481(15) 0.0125(10) 0.0432(14) 0.0144(11) B10 0.0269(12) 0.0354(13) 0.0455(14) 0.0212(11) 0.0253(11) 0.0127(10) B11 0.0194(10) 0.0282(11) 0.0248(10) 0.0095(9) 0.0103(9) 0.0002(9) B12 0.0315(12) 0.0254(11) 0.0389(13) 0.0126(9) 0.0263(11) 0.0110(9) C1 0.0210(9) 0.0162(8) 0.0193(8) 0.0036(6) 0.0135(7) 0.0019(7) C2 0.0201(9) 0.0172(8) 0.0192(8) 0.0041(6) 0.0126(7) 0.0017(7) C3 0.0235(9) 0.0174(8) 0.0210(8) 0.0041(7) 0.0164(8) 0.0045(7) C4 0.0223(9) 0.0159(8) 0.0194(8) -0.0019(6) 0.0138(7) -0.0034(7) C5 0.053(3) 0.0255(18) 0.065(3) -0.0116(19) 0.014(2) -0.0012(17) C5' 0.052(5) 0.039(4) 0.056(5) -0.002(4) 0.021(4) -0.012(3) C6 0.0324(19) 0.0363(19) 0.083(3) 0.000 0.029(2) 0.000 O6 0.0234(17) 0.074(3) 0.054(2) 0.0132(19) 0.0155(18) 0.0010(18) _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 O1 1.9590(13) . ? Cu1 O4 1.9596(13) 4_545 ? Cu1 O2 1.9637(13) 7_556 ? Cu1 O3 1.9643(13) 6_566 ? Cu1 O5 2.1354(15) . ? Cu1 Cu1 2.6517(4) 7_556 ? O1 C3 1.246(2) . ? O2 C3 1.244(2) . ? O2 Cu1 1.9637(13) 7_556 ? O3 C4 1.243(2) . ? O3 Cu1 1.9642(13) 6_565 ? O4 C4 1.249(2) . ? O4 Cu1 1.9597(13) 4 ? O5 C5 1.416(5) . ? O5 C5' 1.439(11) . ? O5 H5' 0.803(17) . ? B3 C1 1.704(3) . ? B3 C2 1.704(3) . ? B3 B4 1.761(3) . ? B3 B8 1.767(3) . ? B3 B7 1.800(3) . ? B3 H3 1.1200 . ? B4 C1 1.720(3) . ? B4 B8 1.770(3) . ? B4 B9 1.777(4) . ? B4 B5 1.787(4) . ? B4 H4 1.1200 . ? B5 C1 1.709(3) . ? B5 B10 1.774(3) . ? B5 B9 1.776(3) . ? B5 B6 1.781(3) . ? B5 H5 1.1200 . ? B6 C1 1.722(3) . ? B6 B7 1.770(3) . ? B6 B11 1.774(3) . ? B6 B10 1.775(3) . ? B6 H6 1.1200 . ? B7 C1 1.699(2) . ? B7 C2 1.708(3) . ? B7 B11 1.777(3) . ? B7 H7 1.1200 . ? B8 C2 1.708(3) . ? B8 B9 1.788(4) . ? B8 B12 1.789(4) . ? B8 H8 1.1200 . ? B9 B12 1.777(3) . ? B9 B10 1.783(4) . ? B9 H9 1.1200 . ? B10 B12 1.775(3) . ? B10 B11 1.779(3) . ? B10 H10 1.1200 . ? B11 C2 1.720(3) . ? B11 B12 1.771(3) . ? B11 H11 1.1200 . ? B12 C2 1.719(3) . ? B12 H12 1.1200 . ? C1 C3 1.525(2) . ? C2 C4 1.523(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C5' H5'1 0.9800 . ? C5' H5'2 0.9800 . ? C5' H5'3 0.9800 . ? C6 O6 1.470(5) . ? C6 O6 1.470(5) 2 ? C6 H6A 1.010(18) . ? C6 H6B 1.024(19) . ? O6 O6 1.265(8) 2 ? O6 H6B 1.11(7) . ? O6 H6' 0.85(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 O1 Cu1 O4 90.15(7) . 4_545 ? O1 Cu1 O2 167.68(6) . 7_556 ? O4 Cu1 O2 88.45(6) 4_545 7_556 ? O1 Cu1 O3 88.85(7) . 6_566 ? O4 Cu1 O3 167.81(6) 4_545 6_566 ? O2 Cu1 O3 89.94(7) 7_556 6_566 ? O1 Cu1 O5 93.32(6) . . ? O4 Cu1 O5 98.32(6) 4_545 . ? O2 Cu1 O5 98.99(6) 7_556 . ? O3 Cu1 O5 93.86(6) 6_566 . ? O1 Cu1 Cu1 82.01(4) . 7_556 ? O4 Cu1 Cu1 84.82(4) 4_545 7_556 ? O2 Cu1 Cu1 85.67(4) 7_556 7_556 ? O3 Cu1 Cu1 83.01(4) 6_566 7_556 ? O5 Cu1 Cu1 174.41(4) . 7_556 ? C3 O1 Cu1 124.70(12) . . ? C3 O2 Cu1 120.17(12) . 7_556 ? C4 O3 Cu1 123.28(12) . 6_565 ? C4 O4 Cu1 121.23(12) . 4 ? C5 O5 C5' 27.9(5) . . ? C5 O5 Cu1 121.3(2) . . ? C5' O5 Cu1 120.6(5) . . ? C5 O5 H5' 106(2) . . ? C5' O5 H5' 120(2) . . ? Cu1 O5 H5' 119(2) . . ? C1 B3 C2 100.80(14) . . ? C1 B3 B4 59.49(12) . . ? C2 B3 B4 104.96(15) . . ? C1 B3 B8 105.34(15) . . ? C2 B3 B8 58.93(12) . . ? B4 B3 B8 60.24(12) . . ? C1 B3 B7 57.91(10) . . ? C2 B3 B7 58.28(11) . . ? B4 B3 B7 107.98(15) . . ? B8 B3 B7 107.90(15) . . ? C1 B3 H3 125.4 . . ? C2 B3 H3 125.7 . . ? B4 B3 H3 121.6 . . ? B8 B3 H3 121.7 . . ? B7 B3 H3 121.7 . . ? C1 B4 B3 58.60(11) . . ? C1 B4 B8 104.51(14) . . ? B3 B4 B8 60.05(12) . . ? C1 B4 B9 104.31(17) . . ? B3 B4 B9 108.41(15) . . ? B8 B4 B9 60.54(14) . . ? C1 B4 B5 58.30(12) . . ? B3 B4 B5 107.78(15) . . ? B8 B4 B5 108.10(17) . . ? B9 B4 B5 59.78(14) . . ? C1 B4 H4 125.2 . . ? B3 B4 H4 121.4 . . ? B8 B4 H4 122.1 . . ? B9 B4 H4 122.2 . . ? B5 B4 H4 121.7 . . ? C1 B5 B10 104.94(15) . . ? C1 B5 B9 104.78(15) . . ? B10 B5 B9 60.29(15) . . ? C1 B5 B6 59.08(11) . . ? B10 B5 B6 59.92(14) . . ? B9 B5 B6 108.30(15) . . ? C1 B5 B4 58.88(12) . . ? B10 B5 B4 108.24(15) . . ? B9 B5 B4 59.82(15) . . ? B6 B5 B4 108.57(14) . . ? C1 B5 H5 124.6 . . ? B10 B5 H5 122.2 . . ? B9 B5 H5 122.3 . . ? B6 B5 H5 121.1 . . ? B4 B5 H5 121.3 . . ? C1 B6 B7 58.19(11) . . ? C1 B6 B11 104.24(14) . . ? B7 B6 B11 60.20(12) . . ? C1 B6 B10 104.38(17) . . ? B7 B6 B10 108.22(15) . . ? B11 B6 B10 60.16(13) . . ? C1 B6 B5 58.40(12) . . ? B7 B6 B5 107.45(16) . . ? B11 B6 B5 107.73(16) . . ? B10 B6 B5 59.86(13) . . ? C1 B6 H6 125.3 . . ? B7 B6 H6 121.6 . . ? B11 B6 H6 122.4 . . ? B10 B6 H6 122.2 . . ? B5 B6 H6 121.8 . . ? C1 B7 C2 100.86(13) . . ? C1 B7 B6 59.48(11) . . ? C2 B7 B6 105.07(14) . . ? C1 B7 B11 105.07(14) . . ? C2 B7 B11 59.09(11) . . ? B6 B7 B11 60.00(12) . . ? C1 B7 B3 58.21(11) . . ? C2 B7 B3 58.06(11) . . ? B6 B7 B3 108.21(14) . . ? B11 B7 B3 107.78(14) . . ? C1 B7 H7 125.4 . . ? C2 B7 H7 125.6 . . ? B6 B7 H7 121.6 . . ? B11 B7 H7 121.9 . . ? B3 B7 H7 121.7 . . ? C2 B8 B3 58.71(11) . . ? C2 B8 B4 104.40(15) . . ? B3 B8 B4 59.72(12) . . ? C2 B8 B9 104.40(17) . . ? B3 B8 B9 107.64(15) . . ? B4 B8 B9 59.91(13) . . ? C2 B8 B12 58.81(12) . . ? B3 B8 B12 107.93(15) . . ? B4 B8 B12 107.54(17) . . ? B9 B8 B12 59.58(14) . . ? C2 B8 H8 124.8 . . ? B3 B8 H8 121.6 . . ? B4 B8 H8 122.7 . . ? B9 B8 H8 122.7 . . ? B12 B8 H8 121.6 . . ? B5 B9 B4 60.40(13) . . ? B5 B9 B12 107.45(17) . . ? B4 B9 B12 107.78(16) . . ? B5 B9 B10 59.80(14) . . ? B4 B9 B10 108.31(16) . . ? B12 B9 B10 59.82(14) . . ? B5 B9 B8 107.80(16) . . ? B4 B9 B8 59.55(14) . . ? B12 B9 B8 60.24(13) . . ? B10 B9 B8 108.19(16) . . ? B5 B9 H9 121.9 . . ? B4 B9 H9 121.6 . . ? B12 B9 H9 122.0 . . ? B10 B9 H9 121.6 . . ? B8 B9 H9 121.8 . . ? B5 B10 B6 60.22(13) . . ? B5 B10 B12 107.63(18) . . ? B6 B10 B12 107.79(16) . . ? B5 B10 B11 107.79(16) . . ? B6 B10 B11 59.88(13) . . ? B12 B10 B11 59.76(13) . . ? B5 B10 B9 59.91(14) . . ? B6 B10 B9 108.24(17) . . ? B12 B10 B9 59.93(14) . . ? B11 B10 B9 107.83(17) . . ? B5 B10 H10 121.8 . . ? B6 B10 H10 121.6 . . ? B12 B10 H10 122.0 . . ? B11 B10 H10 121.9 . . ? B9 B10 H10 121.7 . . ? C2 B11 B12 58.97(12) . . ? C2 B11 B6 104.43(14) . . ? B12 B11 B6 108.05(16) . . ? C2 B11 B7 58.46(11) . . ? B12 B11 B7 108.04(16) . . ? B6 B11 B7 59.80(12) . . ? C2 B11 B10 104.71(16) . . ? B12 B11 B10 60.02(14) . . ? B6 B11 B10 59.96(12) . . ? B7 B11 B10 107.74(15) . . ? C2 B11 H11 124.8 . . ? B12 B11 H11 121.3 . . ? B6 B11 H11 122.5 . . ? B7 B11 H11 121.7 . . ? B10 B11 H11 122.4 . . ? C2 B12 B11 59.04(12) . . ? C2 B12 B10 104.92(15) . . ? B11 B12 B10 60.22(14) . . ? C2 B12 B9 104.44(16) . . ? B11 B12 B9 108.46(16) . . ? B10 B12 B9 60.25(15) . . ? C2 B12 B8 58.25(12) . . ? B11 B12 B8 108.34(15) . . ? B10 B12 B8 108.49(16) . . ? B9 B12 B8 60.19(15) . . ? C2 B12 H12 125.0 . . ? B11 B12 H12 121.1 . . ? B10 B12 H12 122.0 . . ? B9 B12 H12 122.3 . . ? B8 B12 H12 121.4 . . ? C3 C1 B7 118.25(14) . . ? C3 C1 B3 116.80(15) . . ? B7 C1 B3 63.88(11) . . ? C3 C1 B5 118.03(14) . . ? B7 C1 B5 114.28(14) . . ? B3 C1 B5 114.25(14) . . ? C3 C1 B4 116.72(14) . . ? B7 C1 B4 114.85(13) . . ? B3 C1 B4 61.90(12) . . ? B5 C1 B4 62.82(13) . . ? C3 C1 B6 118.91(15) . . ? B7 C1 B6 62.33(12) . . ? B3 C1 B6 115.19(13) . . ? B5 C1 B6 62.52(13) . . ? B4 C1 B6 114.64(15) . . ? C4 C2 B3 117.52(15) . . ? C4 C2 B8 118.79(15) . . ? B3 C2 B8 62.36(12) . . ? C4 C2 B7 116.37(14) . . ? B3 C2 B7 63.66(11) . . ? B8 C2 B7 115.14(13) . . ? C4 C2 B12 119.08(14) . . ? B3 C2 B12 114.29(14) . . ? B8 C2 B12 62.94(14) . . ? B7 C2 B12 113.81(14) . . ? C4 C2 B11 117.05(14) . . ? B3 C2 B11 115.13(14) . . ? B8 C2 B11 114.66(15) . . ? B7 C2 B11 62.46(12) . . ? B12 C2 B11 61.98(13) . . ? O2 C3 O1 127.29(17) . . ? O2 C3 C1 117.04(16) . . ? O1 C3 C1 115.66(16) . . ? O3 C4 O4 127.58(16) . . ? O3 C4 C2 116.13(15) . . ? O4 C4 C2 116.29(16) . . ? O5 C5 H5A 109.5 . . ? O5 C5 H5B 109.5 . . ? O5 C5 H5C 109.5 . . ? O5 C5' H5'1 109.5 . . ? O5 C5' H5'2 109.5 . . ? H5'1 C5' H5'2 109.5 . . ? O5 C5' H5'3 109.5 . . ? H5'1 C5' H5'3 109.5 . . ? H5'2 C5' H5'3 109.5 . . ? O6 C6 O6 50.9(4) . 2 ? O6 C6 H6A 118.1(19) . . ? O6 C6 H6A 115.5(19) 2 . ? O6 C6 H6B 49(4) . . ? O6 C6 H6B 100(4) 2 . ? H6A C6 H6B 104(2) . . ? O6 O6 C6 64.53(19) 2 . ? O6 O6 H6B 108.4(11) 2 . ? C6 O6 H6B 44.0(10) . . ? O6 O6 H6' 91(5) 2 . ? C6 O6 H6' 105(2) . . ? H6B O6 H6' 109(5) . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.013 578.6 41.6 2 0.500 0.500 0.199 578.0 41.6 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.91 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.370 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.070 # Attachment '- 3_rev_Compound-3.cif' data_mo_10328a _database_code_depnum_ccdc_archive 'CCDC 873636' #TrackingRef '- 3_rev_Compound-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H21 B10 Cu N O6' _chemical_formula_weight 398.90 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' B B 0.0013 0.0007 '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' _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 11.7400(10) _cell_length_b 12.6840(11) _cell_length_c 13.5746(12) _cell_angle_alpha 90.00 _cell_angle_beta 113.3010(10) _cell_angle_gamma 90.00 _cell_volume 1856.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7645 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 27.80 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 1.199 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5854 _exptl_absorpt_correction_T_max 0.7536 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.54 _diffrn_reflns_number 13552 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0221 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 27.81 _reflns_number_total 4381 _reflns_number_gt 3793 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0500P)^2^+0.9652P] 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 4381 _refine_ls_number_parameters 252 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0891 _refine_ls_wR_factor_gt 0.0834 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 Cu1 Cu 0.414247(18) 0.552814(15) 0.021635(16) 0.01709(8) Uani 1 1 d . . . O1 O 0.53883(13) 0.66520(11) 0.05177(13) 0.0331(3) Uani 1 1 d . . . O2 O 0.68233(13) 0.57931(10) 0.01345(13) 0.0316(3) Uani 1 1 d . . . O3 O 0.85429(14) 0.91253(12) 0.36830(11) 0.0315(3) Uani 1 1 d . . . O4 O 0.99992(13) 0.99786(12) 0.33214(11) 0.0324(3) Uani 1 1 d . . . O5 O 0.28808(15) 0.65099(11) 0.05058(13) 0.0348(3) Uani 1 1 d D . . H5' H 0.237(3) 0.624(3) 0.069(3) 0.069(10) Uiso 1 1 d D . . B3 B 0.70627(18) 0.84276(15) 0.15340(16) 0.0212(4) Uani 1 1 d . . . H3 H 0.6550 0.8266 0.2060 0.025 Uiso 1 1 calc R . . B4 B 0.6270(2) 0.87499(16) 0.01705(18) 0.0284(4) Uani 1 1 d . . . H4 H 0.5233 0.8796 -0.0212 0.034 Uiso 1 1 calc R . . B5 B 0.7159(2) 0.82382(18) -0.05319(18) 0.0319(5) Uani 1 1 d . . . H5 H 0.6702 0.7944 -0.1376 0.038 Uiso 1 1 calc R . . B6 B 0.8507(2) 0.76092(18) 0.04134(18) 0.0288(4) Uani 1 1 d . . . H6 H 0.8932 0.6906 0.0192 0.035 Uiso 1 1 calc R . . B7 B 0.84539(18) 0.77204(15) 0.16934(16) 0.0218(4) Uani 1 1 d . . . H7 H 0.8853 0.7100 0.2324 0.026 Uiso 1 1 calc R . . B8 B 0.7182(2) 0.97116(17) 0.10887(18) 0.0276(4) Uani 1 1 d . . . H8 H 0.6766 1.0408 0.1331 0.033 Uiso 1 1 calc R . . B9 B 0.7231(3) 0.95972(18) -0.02031(19) 0.0376(6) Uani 1 1 d . . . H9 H 0.6828 1.0218 -0.0833 0.045 Uiso 1 1 calc R . . B10 B 0.8608(3) 0.8897(2) -0.00558(19) 0.0374(6) Uani 1 1 d . . . H10 H 0.9111 0.9056 -0.0589 0.045 Uiso 1 1 calc R . . B11 B 0.9410(2) 0.85802(18) 0.13197(19) 0.0289(4) Uani 1 1 d . . . H11 H 1.0446 0.8537 0.1710 0.035 Uiso 1 1 calc R . . B12 B 0.8626(2) 0.98037(18) 0.09425(18) 0.0305(5) Uani 1 1 d . . . H12 H 0.9152 1.0564 0.1086 0.037 Uiso 1 1 calc R . . C1 C 0.71197(16) 0.76068(13) 0.05693(14) 0.0203(3) Uani 1 1 d . . . C2 C 0.84670(16) 0.90406(13) 0.19256(14) 0.0202(3) Uani 1 1 d . . . C3 C 0.63798(16) 0.65840(13) 0.03944(13) 0.0208(3) Uani 1 1 d . . . C4 C 0.90619(16) 0.94161(12) 0.30826(14) 0.0206(3) Uani 1 1 d . . . C5 C 0.2420(3) 0.7461(2) -0.0067(2) 0.0552(7) Uani 1 1 d . . . H5A H 0.3104 0.7962 0.0083 0.083 Uiso 1 1 calc R . . H5B H 0.1794 0.7765 0.0158 0.083 Uiso 1 1 calc R . . H5C H 0.2044 0.7311 -0.0838 0.083 Uiso 1 1 calc R . . O6 O 0.8542(3) 0.4257(2) 0.8658(3) 0.0963(10) Uani 1 1 d . . . N1 N 0.9158(2) 0.57321(17) 0.81141(18) 0.0458(5) Uani 1 1 d . . . C6 C 0.8377(3) 0.5189(3) 0.8367(3) 0.0639(8) Uani 1 1 d . . . H6A H 0.7637 0.5525 0.8326 0.077 Uiso 1 1 calc R . . C7 C 1.0290(3) 0.5247(3) 0.8150(3) 0.0597(8) Uani 1 1 d . . . H7A H 1.0284 0.4494 0.8312 0.090 Uiso 1 1 calc R . . H7B H 1.1005 0.5586 0.8709 0.090 Uiso 1 1 calc R . . H7C H 1.0348 0.5332 0.7454 0.090 Uiso 1 1 calc R . . C8 C 0.8941(3) 0.6830(2) 0.7797(3) 0.0646(8) Uani 1 1 d . . . H8A H 0.8100 0.7029 0.7708 0.097 Uiso 1 1 calc R . . H8B H 0.9035 0.6931 0.7117 0.097 Uiso 1 1 calc R . . H8C H 0.9544 0.7272 0.8352 0.097 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01826(12) 0.01313(11) 0.01847(12) 0.00073(7) 0.00574(8) 0.00009(7) O1 0.0315(7) 0.0227(6) 0.0508(9) -0.0107(6) 0.0223(7) -0.0094(6) O2 0.0296(7) 0.0177(6) 0.0496(9) -0.0066(6) 0.0178(7) -0.0052(5) O3 0.0360(7) 0.0372(8) 0.0215(6) -0.0074(6) 0.0113(6) -0.0148(6) O4 0.0326(7) 0.0401(8) 0.0235(7) -0.0093(6) 0.0099(6) -0.0161(6) O5 0.0397(8) 0.0234(7) 0.0511(9) 0.0066(6) 0.0284(7) 0.0098(6) B3 0.0212(9) 0.0175(8) 0.0224(9) -0.0026(7) 0.0060(7) -0.0021(7) B4 0.0300(10) 0.0186(9) 0.0268(10) 0.0024(8) 0.0008(9) -0.0005(8) B5 0.0454(13) 0.0277(11) 0.0207(10) -0.0008(8) 0.0108(9) -0.0138(10) B6 0.0319(11) 0.0286(10) 0.0310(11) -0.0101(9) 0.0179(9) -0.0104(9) B7 0.0212(9) 0.0175(8) 0.0242(9) -0.0029(7) 0.0063(7) -0.0014(7) B8 0.0280(10) 0.0186(9) 0.0276(10) -0.0010(8) 0.0019(8) 0.0000(8) B9 0.0545(15) 0.0242(10) 0.0244(11) 0.0040(9) 0.0051(10) -0.0132(10) B10 0.0534(15) 0.0363(12) 0.0286(11) -0.0094(10) 0.0228(11) -0.0229(11) B11 0.0282(10) 0.0298(11) 0.0326(11) -0.0099(9) 0.0163(9) -0.0096(9) B12 0.0413(12) 0.0247(10) 0.0248(10) -0.0004(8) 0.0122(9) -0.0138(9) C1 0.0231(8) 0.0152(7) 0.0205(8) -0.0010(6) 0.0064(7) -0.0036(6) C2 0.0229(8) 0.0165(7) 0.0199(8) -0.0018(6) 0.0069(7) -0.0029(6) C3 0.0236(8) 0.0169(7) 0.0181(8) 0.0003(6) 0.0043(6) -0.0040(6) C4 0.0220(8) 0.0156(7) 0.0208(8) -0.0019(6) 0.0048(7) 0.0020(6) C5 0.0671(18) 0.0332(12) 0.0617(17) 0.0068(12) 0.0215(14) 0.0222(12) O6 0.104(2) 0.0726(16) 0.164(3) 0.0358(18) 0.108(2) 0.0205(15) N1 0.0494(12) 0.0485(12) 0.0423(11) 0.0011(9) 0.0213(10) 0.0072(9) C6 0.0635(18) 0.0663(19) 0.083(2) 0.0075(17) 0.0522(18) 0.0091(16) C7 0.0476(15) 0.0567(16) 0.082(2) 0.0116(16) 0.0331(15) 0.0034(13) C8 0.077(2) 0.0510(16) 0.068(2) 0.0062(14) 0.0320(17) 0.0125(15) _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 O4 1.9644(13) 2_645 ? Cu1 O3 1.9652(14) 4_575 ? Cu1 O1 1.9660(13) . ? Cu1 O2 1.9733(13) 3_665 ? Cu1 O5 2.0879(14) . ? Cu1 Cu1 2.6701(4) 3_665 ? O1 C3 1.243(2) . ? O2 C3 1.244(2) . ? O2 Cu1 1.9733(13) 3_665 ? O3 C4 1.251(2) . ? O3 Cu1 1.9652(14) 4_676 ? O4 C4 1.242(2) . ? O4 Cu1 1.9644(13) 2_655 ? O5 C5 1.421(3) . ? O5 H5' 0.812(18) . ? B3 C1 1.695(3) . ? B3 C2 1.706(3) . ? B3 B4 1.760(3) . ? B3 B8 1.762(3) . ? B3 B7 1.800(3) . ? B3 H3 1.1200 . ? B4 C1 1.721(3) . ? B4 B8 1.770(3) . ? B4 B9 1.771(3) . ? B4 B5 1.791(3) . ? B4 H4 1.1200 . ? B5 C1 1.713(3) . ? B5 B10 1.771(3) . ? B5 B9 1.774(3) . ? B5 B6 1.783(4) . ? B5 H5 1.1200 . ? B6 C1 1.723(3) . ? B6 B11 1.767(3) . ? B6 B7 1.769(3) . ? B6 B10 1.775(3) . ? B6 H6 1.1200 . ? B7 C2 1.703(3) . ? B7 C1 1.706(3) . ? B7 B11 1.777(3) . ? B7 H7 1.1200 . ? B8 C2 1.713(3) . ? B8 B9 1.783(4) . ? B8 B12 1.787(3) . ? B8 H8 1.1200 . ? B9 B12 1.776(3) . ? B9 B10 1.784(4) . ? B9 H9 1.1200 . ? B10 B12 1.771(3) . ? B10 B11 1.773(4) . ? B10 H10 1.1200 . ? B11 C2 1.721(3) . ? B11 B12 1.773(3) . ? B11 H11 1.1200 . ? B12 C2 1.717(3) . ? B12 H12 1.1200 . ? C1 C3 1.527(2) . ? C2 C4 1.521(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? O6 C6 1.237(4) . ? N1 C6 1.297(4) . ? N1 C7 1.448(3) . ? N1 C8 1.450(4) . ? C6 H6A 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 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 O4 Cu1 O3 167.23(6) 2_645 4_575 ? O4 Cu1 O1 90.29(7) 2_645 . ? O3 Cu1 O1 89.06(7) 4_575 . ? O4 Cu1 O2 87.63(7) 2_645 3_665 ? O3 Cu1 O2 90.20(7) 4_575 3_665 ? O1 Cu1 O2 167.20(6) . 3_665 ? O4 Cu1 O5 98.05(6) 2_645 . ? O3 Cu1 O5 94.72(6) 4_575 . ? O1 Cu1 O5 93.05(6) . . ? O2 Cu1 O5 99.75(6) 3_665 . ? O4 Cu1 Cu1 85.08(4) 2_645 3_665 ? O3 Cu1 Cu1 82.22(4) 4_575 3_665 ? O1 Cu1 Cu1 81.14(4) . 3_665 ? O2 Cu1 Cu1 86.10(4) 3_665 3_665 ? O5 Cu1 Cu1 173.44(4) . 3_665 ? C3 O1 Cu1 125.52(12) . . ? C3 O2 Cu1 119.23(12) . 3_665 ? C4 O3 Cu1 124.16(12) . 4_676 ? C4 O4 Cu1 120.99(12) . 2_655 ? C5 O5 Cu1 123.22(15) . . ? C5 O5 H5' 111(3) . . ? Cu1 O5 H5' 119(2) . . ? C1 B3 C2 101.07(13) . . ? C1 B3 B4 59.74(11) . . ? C2 B3 B4 105.40(14) . . ? C1 B3 B8 105.65(14) . . ? C2 B3 B8 59.17(11) . . ? B4 B3 B8 60.34(12) . . ? C1 B3 B7 58.36(11) . . ? C2 B3 B7 58.04(10) . . ? B4 B3 B7 108.63(14) . . ? B8 B3 B7 108.08(14) . . ? C1 B3 H3 125.1 . . ? C2 B3 H3 125.6 . . ? B4 B3 H3 121.3 . . ? B8 B3 H3 121.6 . . ? B7 B3 H3 121.5 . . ? C1 B4 B3 58.26(11) . . ? C1 B4 B8 104.19(14) . . ? B3 B4 B8 59.90(12) . . ? C1 B4 B9 104.21(17) . . ? B3 B4 B9 108.08(15) . . ? B8 B4 B9 60.46(13) . . ? C1 B4 B5 58.32(12) . . ? B3 B4 B5 107.38(15) . . ? B8 B4 B5 107.87(16) . . ? B9 B4 B5 59.73(14) . . ? C1 B4 H4 125.3 . . ? B3 B4 H4 121.7 . . ? B8 B4 H4 122.3 . . ? B9 B4 H4 122.3 . . ? B5 B4 H4 121.8 . . ? C1 B5 B10 104.83(15) . . ? C1 B5 B9 104.46(15) . . ? B10 B5 B9 60.43(15) . . ? C1 B5 B6 59.02(12) . . ? B10 B5 B6 59.91(14) . . ? B9 B5 B6 108.27(16) . . ? C1 B5 B4 58.80(12) . . ? B10 B5 B4 108.19(16) . . ? B9 B5 B4 59.58(14) . . ? B6 B5 B4 108.48(15) . . ? C1 B5 H5 124.8 . . ? B10 B5 H5 122.2 . . ? B9 B5 H5 122.4 . . ? B6 B5 H5 121.2 . . ? B4 B5 H5 121.4 . . ? C1 B6 B11 104.58(14) . . ? C1 B6 B7 58.50(11) . . ? B11 B6 B7 60.33(12) . . ? C1 B6 B10 104.25(16) . . ? B11 B6 B10 60.08(13) . . ? B7 B6 B10 108.21(15) . . ? C1 B6 B5 58.46(12) . . ? B11 B6 B5 107.84(16) . . ? B7 B6 B5 107.79(15) . . ? B10 B6 B5 59.72(14) . . ? C1 B6 H6 125.1 . . ? B11 B6 H6 122.2 . . ? B7 B6 H6 121.3 . . ? B10 B6 H6 122.5 . . ? B5 B6 H6 121.7 . . ? C2 B7 C1 100.75(13) . . ? C2 B7 B6 105.01(14) . . ? C1 B7 B6 59.41(12) . . ? C2 B7 B11 59.25(11) . . ? C1 B7 B11 104.86(14) . . ? B6 B7 B11 59.79(12) . . ? C2 B7 B3 58.23(10) . . ? C1 B7 B3 57.74(10) . . ? B6 B7 B3 107.72(15) . . ? B11 B7 B3 107.79(14) . . ? C2 B7 H7 125.4 . . ? C1 B7 H7 125.6 . . ? B6 B7 H7 121.8 . . ? B11 B7 H7 121.9 . . ? B3 B7 H7 121.9 . . ? C2 B8 B3 58.80(11) . . ? C2 B8 B4 104.68(14) . . ? B3 B8 B4 59.76(12) . . ? C2 B8 B9 104.44(16) . . ? B3 B8 B9 107.47(15) . . ? B4 B8 B9 59.81(13) . . ? C2 B8 B12 58.73(12) . . ? B3 B8 B12 107.84(15) . . ? B4 B8 B12 107.65(16) . . ? B9 B8 B12 59.67(14) . . ? C2 B8 H8 124.7 . . ? B3 B8 H8 121.7 . . ? B4 B8 H8 122.5 . . ? B9 B8 H8 122.7 . . ? B12 B8 H8 121.6 . . ? B4 B9 B5 60.69(13) . . ? B4 B9 B12 108.05(16) . . ? B5 B9 B12 107.40(18) . . ? B4 B9 B8 59.72(13) . . ? B5 B9 B8 108.04(15) . . ? B12 B9 B8 60.26(13) . . ? B4 B9 B10 108.50(16) . . ? B5 B9 B10 59.71(14) . . ? B12 B9 B10 59.65(14) . . ? B8 B9 B10 108.08(17) . . ? B4 B9 H9 121.3 . . ? B5 B9 H9 121.8 . . ? B12 B9 H9 122.0 . . ? B8 B9 H9 121.7 . . ? B10 B9 H9 121.7 . . ? B12 B10 B5 107.76(18) . . ? B12 B10 B11 60.05(13) . . ? B5 B10 B11 108.09(15) . . ? B12 B10 B6 107.78(15) . . ? B5 B10 B6 60.37(13) . . ? B11 B10 B6 59.75(13) . . ? B12 B10 B9 59.94(14) . . ? B5 B10 B9 59.87(14) . . ? B11 B10 B9 108.14(16) . . ? B6 B10 B9 108.19(16) . . ? B12 B10 H10 121.9 . . ? B5 B10 H10 121.7 . . ? B11 B10 H10 121.7 . . ? B6 B10 H10 121.7 . . ? B9 B10 H10 121.6 . . ? C2 B11 B6 104.29(14) . . ? C2 B11 B10 104.59(17) . . ? B6 B11 B10 60.17(13) . . ? C2 B11 B12 58.84(12) . . ? B6 B11 B12 107.99(17) . . ? B10 B11 B12 59.90(14) . . ? C2 B11 B7 58.23(11) . . ? B6 B11 B7 59.87(12) . . ? B10 B11 B7 107.91(15) . . ? B12 B11 B7 107.77(15) . . ? C2 B11 H11 125.0 . . ? B6 B11 H11 122.4 . . ? B10 B11 H11 122.3 . . ? B12 B11 H11 121.5 . . ? B7 B11 H11 121.7 . . ? C2 B12 B10 104.88(15) . . ? C2 B12 B11 59.07(12) . . ? B10 B12 B11 60.05(14) . . ? C2 B12 B9 104.56(15) . . ? B10 B12 B9 60.41(15) . . ? B11 B12 B9 108.50(16) . . ? C2 B12 B8 58.50(11) . . ? B10 B12 B8 108.53(16) . . ? B11 B12 B8 108.52(15) . . ? B9 B12 B8 60.07(14) . . ? C2 B12 H12 124.9 . . ? B10 B12 H12 122.1 . . ? B11 B12 H12 121.1 . . ? B9 B12 H12 122.2 . . ? B8 B12 H12 121.3 . . ? C3 C1 B3 116.62(14) . . ? C3 C1 B7 118.38(14) . . ? B3 C1 B7 63.90(11) . . ? C3 C1 B5 118.16(14) . . ? B3 C1 B5 114.21(14) . . ? B7 C1 B5 114.13(14) . . ? C3 C1 B4 116.33(14) . . ? B3 C1 B4 62.00(12) . . ? B7 C1 B4 115.01(13) . . ? B5 C1 B4 62.88(13) . . ? C3 C1 B6 119.32(14) . . ? B3 C1 B6 114.95(13) . . ? B7 C1 B6 62.09(12) . . ? B5 C1 B6 62.52(13) . . ? B4 C1 B6 114.72(15) . . ? C4 C2 B7 117.77(14) . . ? C4 C2 B3 117.17(14) . . ? B7 C2 B3 63.73(11) . . ? C4 C2 B8 116.96(14) . . ? B7 C2 B8 115.13(14) . . ? B3 C2 B8 62.03(12) . . ? C4 C2 B12 118.64(14) . . ? B7 C2 B12 113.97(14) . . ? B3 C2 B12 113.78(14) . . ? B8 C2 B12 62.77(13) . . ? C4 C2 B11 118.70(15) . . ? B7 C2 B11 62.51(11) . . ? B3 C2 B11 114.92(13) . . ? B8 C2 B11 114.56(15) . . ? B12 C2 B11 62.09(13) . . ? O1 C3 O2 127.85(16) . . ? O1 C3 C1 115.20(15) . . ? O2 C3 C1 116.94(15) . . ? O4 C4 O3 127.51(17) . . ? O4 C4 C2 116.55(16) . . ? O3 C4 C2 115.94(15) . . ? O5 C5 H5A 109.5 . . ? O5 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O5 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C6 N1 C7 120.0(3) . . ? C6 N1 C8 122.0(3) . . ? C7 N1 C8 118.0(2) . . ? O6 C6 N1 123.7(3) . . ? O6 C6 H6A 118.2 . . ? N1 C6 H6A 118.2 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5' O6 0.812(18) 1.753(19) 2.555(3) 169(4) 3_666 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.81 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.445 _refine_diff_density_min -0.315 _refine_diff_density_rms 0.070 # Attachment '- 4th-revised Compound-4.cif' data_mo_10503a _database_code_depnum_ccdc_archive 'CCDC 873637' #TrackingRef '- 4th-revised Compound-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H20 B10 Cu N2 O4' _chemical_formula_weight 451.96 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 9.5924(17) _cell_length_b 10.2168(18) _cell_length_c 11.281(2) _cell_angle_alpha 74.845(3) _cell_angle_beta 82.169(3) _cell_angle_gamma 80.761(3) _cell_volume 1048.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3102 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 27.53 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 458 _exptl_absorpt_coefficient_mu 1.066 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7992 _exptl_absorpt_correction_T_max 0.9195 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7323 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0446 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.00 _reflns_number_total 4478 _reflns_number_gt 3702 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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. In this data, 11 ISOR instructions were used to restrain atoms in two disordered pyridine molecule coordinated with Cu1 so that there were 66 restraints. ; _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^)+(0.1522P)^2^+0.2367P] 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 4478 _refine_ls_number_parameters 315 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.0749 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.2063 _refine_ls_wR_factor_gt 0.1649 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.049 _refine_ls_shift/su_mean 0.005 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 Cu1 Cu 0.59160(5) 0.59284(4) 0.60838(4) 0.0224(2) Uani 1 1 d . . . N1 N 0.4433(4) 0.5926(3) 0.7542(3) 0.0233(6) Uani 1 1 d . A . O1 O 0.6301(3) 0.7766(3) 0.6159(3) 0.0277(6) Uani 1 1 d . A . O2 O 0.7751(3) 0.6454(3) 0.7506(3) 0.0351(7) Uani 1 1 d . A . O3 O 0.5860(3) 1.2949(3) 0.5102(3) 0.0274(6) Uani 1 1 d . . . O4 O 0.6222(3) 1.3920(3) 0.6570(3) 0.0329(7) Uani 1 1 d . . . B3 B 0.6071(5) 1.0196(4) 0.7146(4) 0.0234(8) Uani 1 1 d . . . H3 H 0.5027 1.0205 0.6802 0.028 Uiso 1 1 calc R . . B4 B 0.7647(5) 1.0300(4) 0.6128(4) 0.0224(8) Uani 1 1 d . . . H4 H 0.7642 1.0380 0.5119 0.027 Uiso 1 1 calc R . . B5 B 0.9074(5) 0.9353(4) 0.6983(5) 0.0330(10) Uani 1 1 d . . . H5 H 1.0020 0.8796 0.6542 0.040 Uiso 1 1 calc R . . B6 B 0.8357(6) 0.8687(5) 0.8523(5) 0.0391(12) Uani 1 1 d . . . H6 H 0.8844 0.7688 0.9087 0.047 Uiso 1 1 calc R . . B7 B 0.6487(6) 0.9183(5) 0.8610(4) 0.0357(11) Uani 1 1 d . . . H7 H 0.5735 0.8506 0.9226 0.043 Uiso 1 1 calc R . . B8 B 0.8773(5) 1.1175(5) 0.6687(5) 0.0330(10) Uani 1 1 d . . . H8 H 0.9520 1.1837 0.6044 0.040 Uiso 1 1 calc R . . B9 B 0.9181(7) 1.0181(5) 0.8204(6) 0.0500(16) Uani 1 1 d . . . H9 H 1.0208 1.0185 0.8569 0.060 Uiso 1 1 calc R . . B10 B 0.7579(8) 1.0060(6) 0.9198(5) 0.0505(16) Uani 1 1 d . . . H10 H 0.7538 0.9975 1.0212 0.061 Uiso 1 1 calc R . . B11 B 0.6186(6) 1.1007(5) 0.8325(4) 0.0368(12) Uani 1 1 d . . . H11 H 0.5233 1.1572 0.8751 0.044 Uiso 1 1 calc R . . B12 B 0.7864(7) 1.1599(5) 0.8061(5) 0.0405(13) Uani 1 1 d . . . H12 H 0.8019 1.2552 0.8314 0.049 Uiso 1 1 calc R . . C1 C 0.7426(4) 0.8869(4) 0.7279(3) 0.0197(7) Uani 1 1 d . A . C2 C 0.6966(4) 1.1562(3) 0.6852(3) 0.0200(7) Uani 1 1 d . . . C3 C 0.7153(4) 0.7571(4) 0.6964(3) 0.0223(7) Uani 1 1 d . . . C4 C 0.6270(4) 1.2948(3) 0.6087(3) 0.0198(7) Uani 1 1 d . . . C5 C 0.4355(6) 0.4845(4) 0.8499(4) 0.0395(11) Uani 1 1 d . . . H5A H 0.5004 0.4040 0.8490 0.047 Uiso 1 1 calc R A . C6 C 0.3341(8) 0.4858(6) 0.9523(5) 0.0582(16) Uani 1 1 d . A . H6A H 0.3302 0.4070 1.0191 0.070 Uiso 1 1 calc R . . C7 C 0.2435(6) 0.5988(6) 0.9544(5) 0.0534(14) Uani 1 1 d . . . H7A H 0.1739 0.6006 1.0227 0.064 Uiso 1 1 calc R A . C8 C 0.2507(7) 0.7150(6) 0.8561(6) 0.0571(15) Uani 1 1 d . A . H8A H 0.1886 0.7970 0.8575 0.069 Uiso 1 1 calc R . . C9 C 0.3506(5) 0.7070(5) 0.7570(4) 0.0402(11) Uani 1 1 d . . . H9A H 0.3545 0.7841 0.6885 0.048 Uiso 1 1 calc R A . N2 N 0.7350(3) 0.5998(3) 0.4573(3) 0.016(3) Uani 0.64(3) 1 d PGU A 1 C10 C 0.7142(4) 0.7248(5) 0.3715(6) 0.038(2) Uani 0.64(3) 1 d PGU A 1 H10A H 0.6472 0.7968 0.3917 0.046 Uiso 0.64(3) 1 calc PR A 1 C11 C 0.7916(7) 0.7444(12) 0.2561(4) 0.052(3) Uani 0.64(3) 1 d PGU A 1 H11A H 0.7774 0.8298 0.1975 0.062 Uiso 0.64(3) 1 calc PR A 1 C12 C 0.8897(10) 0.6390(14) 0.2266(7) 0.066(4) Uani 0.64(3) 1 d PGU A 1 H12A H 0.9425 0.6524 0.1478 0.079 Uiso 0.64(3) 1 calc PR A 1 C13 C 0.9104(8) 0.5141(10) 0.3125(13) 0.059(3) Uani 0.64(3) 1 d PGU A 1 H13 H 0.9775 0.4420 0.2923 0.071 Uiso 0.64(3) 1 calc PR A 1 C14 C 0.8331(5) 0.4945(3) 0.4278(11) 0.047(3) Uani 0.64(3) 1 d PGU A 1 H14 H 0.8473 0.4091 0.4865 0.057 Uiso 0.64(3) 1 calc PR A 1 N2' N 0.7288(3) 0.6018(3) 0.4630(3) 0.048(8) Uani 0.36(3) 1 d PGU A 2 C10' C 0.7168(4) 0.7018(7) 0.3532(5) 0.032(4) Uani 0.36(3) 1 d PG A 2 H10' H 0.6412 0.7750 0.3473 0.039 Uiso 0.36(3) 1 calc PR A 2 C11' C 0.8156(8) 0.6949(12) 0.2520(3) 0.046(5) Uani 0.36(3) 1 d PGU A 2 H11' H 0.8075 0.7632 0.1769 0.055 Uiso 0.36(3) 1 calc PR A 2 C12' C 0.9263(9) 0.5879(12) 0.2606(10) 0.040(5) Uani 0.36(3) 1 d PGU A 2 H12' H 0.9938 0.5831 0.1915 0.049 Uiso 0.36(3) 1 calc PR A 2 C13' C 0.9382(6) 0.4878(6) 0.3705(15) 0.042(4) Uani 0.36(3) 1 d PGU A 2 H13' H 1.0139 0.4147 0.3764 0.051 Uiso 0.36(3) 1 calc PR A 2 C14' C 0.8395(4) 0.4948(4) 0.4717(10) 0.039(4) Uani 0.36(3) 1 d PGU A 2 H14' H 0.8476 0.4264 0.5467 0.047 Uiso 0.36(3) 1 calc PR A 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 Cu1 0.0315(3) 0.0093(3) 0.0275(3) -0.00495(18) -0.00790(19) -0.00095(17) N1 0.0323(16) 0.0124(14) 0.0278(15) -0.0065(12) -0.0100(13) -0.0016(12) O1 0.0391(15) 0.0158(13) 0.0318(14) -0.0085(11) -0.0125(12) -0.0023(11) O2 0.0459(18) 0.0119(13) 0.0478(18) -0.0044(12) -0.0178(14) 0.0013(12) O3 0.0370(15) 0.0167(13) 0.0291(14) -0.0031(11) -0.0127(11) -0.0010(11) O4 0.0532(19) 0.0115(13) 0.0344(15) -0.0074(11) -0.0091(13) 0.0017(12) B3 0.029(2) 0.0092(17) 0.030(2) -0.0012(15) -0.0004(16) -0.0042(14) B4 0.030(2) 0.0113(18) 0.0246(19) -0.0041(15) -0.0006(16) -0.0003(15) B5 0.024(2) 0.0142(19) 0.059(3) -0.0042(19) -0.012(2) 0.0000(16) B6 0.057(3) 0.022(2) 0.042(3) -0.009(2) -0.027(2) 0.007(2) B7 0.065(3) 0.018(2) 0.020(2) -0.0035(16) 0.001(2) 0.001(2) B8 0.024(2) 0.020(2) 0.056(3) -0.009(2) -0.011(2) 0.0002(16) B9 0.057(3) 0.024(3) 0.075(4) -0.006(3) -0.048(3) -0.001(2) B10 0.100(5) 0.024(3) 0.031(2) -0.004(2) -0.029(3) -0.004(3) B11 0.064(3) 0.020(2) 0.023(2) -0.0077(17) 0.002(2) 0.002(2) B12 0.065(3) 0.022(2) 0.041(3) -0.009(2) -0.032(3) 0.001(2) C1 0.0232(17) 0.0166(16) 0.0197(16) -0.0052(13) -0.0057(13) 0.0008(13) C2 0.0270(18) 0.0119(15) 0.0223(17) -0.0051(13) -0.0056(14) -0.0018(13) C3 0.0252(17) 0.0130(16) 0.0273(17) -0.0054(13) -0.0008(14) 0.0006(13) C4 0.0241(17) 0.0118(16) 0.0220(16) -0.0008(13) -0.0015(13) -0.0041(13) C5 0.062(3) 0.017(2) 0.036(2) -0.0046(17) 0.002(2) -0.0048(19) C6 0.091(5) 0.052(3) 0.032(2) -0.013(2) 0.008(3) -0.018(3) C7 0.060(3) 0.060(4) 0.046(3) -0.023(3) 0.009(2) -0.020(3) C8 0.058(3) 0.050(3) 0.063(4) -0.025(3) -0.003(3) 0.012(3) C9 0.047(3) 0.033(2) 0.038(2) -0.0130(19) -0.010(2) 0.012(2) N2 0.016(3) 0.014(3) 0.019(3) -0.0042(11) -0.0032(9) -0.0048(9) C10 0.035(5) 0.049(5) 0.031(4) -0.008(4) -0.006(3) -0.008(4) C11 0.035(4) 0.064(7) 0.050(6) 0.002(4) -0.001(4) -0.017(4) C12 0.039(6) 0.095(9) 0.054(6) -0.006(6) 0.014(5) -0.015(6) C13 0.036(5) 0.072(8) 0.065(8) -0.026(6) 0.007(5) 0.010(5) C14 0.049(6) 0.036(5) 0.058(6) -0.013(4) 0.004(4) -0.013(4) N2' 0.048(8) 0.048(8) 0.049(8) -0.012(2) -0.0055(13) -0.0071(15) C10' 0.035(9) 0.030(7) 0.034(8) -0.021(7) 0.011(6) -0.001(6) C11' 0.034(8) 0.073(11) 0.026(7) -0.021(7) 0.017(6) -0.001(8) C12' 0.041(8) 0.023(8) 0.055(10) -0.009(6) 0.003(7) -0.003(6) C13' 0.026(6) 0.040(7) 0.059(9) -0.019(6) 0.019(6) -0.006(5) C14' 0.033(7) 0.034(7) 0.062(9) -0.037(7) 0.017(6) -0.013(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2' 1.949(3) . ? Cu1 O4 1.965(3) 1_545 ? Cu1 O1 1.996(3) . ? Cu1 N1 2.023(3) . ? Cu1 N2 2.032(4) . ? Cu1 O3 2.280(3) 2_676 ? N1 C5 1.331(5) . ? N1 C9 1.354(5) . ? O1 C3 1.260(5) . ? O2 C3 1.235(4) . ? O3 C4 1.228(4) . ? O3 Cu1 2.280(3) 2_676 ? O4 C4 1.244(4) . ? O4 Cu1 1.965(3) 1_565 ? B3 C2 1.692(5) . ? B3 C1 1.711(5) . ? B3 B7 1.764(6) . ? B3 B11 1.766(6) . ? B3 B4 1.769(6) . ? B3 H3 1.1200 . ? B4 C2 1.700(5) . ? B4 C1 1.703(5) . ? B4 B8 1.776(6) . ? B4 B5 1.786(6) . ? B4 H4 1.1200 . ? B5 C1 1.696(6) . ? B5 B6 1.777(8) . ? B5 B8 1.785(6) . ? B5 B9 1.815(8) . ? B5 H5 1.1200 . ? B6 C1 1.718(6) . ? B6 B9 1.762(8) . ? B6 B10 1.780(8) . ? B6 B7 1.780(8) . ? B6 H6 1.1200 . ? B7 C1 1.720(6) . ? B7 B10 1.771(8) . ? B7 B11 1.789(6) . ? B7 H7 1.1200 . ? B8 C2 1.711(6) . ? B8 B12 1.792(8) . ? B8 B9 1.805(8) . ? B8 H8 1.1200 . ? B9 B12 1.752(8) . ? B9 B10 1.775(11) . ? B9 H9 1.1200 . ? B10 B11 1.770(8) . ? B10 B12 1.784(8) . ? B10 H10 1.1200 . ? B11 C2 1.717(6) . ? B11 B12 1.770(9) . ? B11 H11 1.1200 . ? B12 C2 1.721(6) . ? B12 H12 1.1200 . ? C1 C3 1.529(5) . ? C2 C4 1.551(5) . ? C5 C6 1.406(7) . ? C5 H5A 0.9500 . ? C6 C7 1.333(9) . ? C6 H6A 0.9500 . ? C7 C8 1.400(9) . ? C7 H7A 0.9500 . ? C8 C9 1.381(8) . ? C8 H8A 0.9500 . ? C9 H9A 0.9500 . ? N2 C10 1.3900 . ? N2 C14 1.3900 . ? C10 C11 1.3900 . ? C10 H10A 0.9500 . ? C11 C12 1.3900 . ? C11 H11A 0.9500 . ? C12 C13 1.3900 . ? C12 H12A 0.9500 . ? C13 C14 1.3900 . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? N2' C10' 1.3900 . ? N2' C14' 1.3900 . ? C10' C11' 1.3900 . ? C10' H10' 0.9500 . ? C11' C12' 1.3900 . ? C11' H11' 0.9500 . ? C12' C13' 1.3900 . ? C12' H12' 0.9500 . ? C13' C14' 1.3900 . ? C13' H13' 0.9500 . ? C14' H14' 0.9500 . ? 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' Cu1 O4 93.06(13) . 1_545 ? N2' Cu1 O1 89.25(12) . . ? O4 Cu1 O1 152.42(13) 1_545 . ? N2' Cu1 N1 176.97(12) . . ? O4 Cu1 N1 89.49(13) 1_545 . ? O1 Cu1 N1 89.23(12) . . ? N2' Cu1 N2 0.6 . . ? O4 Cu1 N2 92.42(12) 1_545 . ? O1 Cu1 N2 89.82(12) . . ? N1 Cu1 N2 177.49(11) . . ? N2' Cu1 O3 91.39(11) . 2_676 ? O4 Cu1 O3 120.48(11) 1_545 2_676 ? O1 Cu1 O3 86.89(10) . 2_676 ? N1 Cu1 O3 85.91(12) . 2_676 ? N2 Cu1 O3 91.72(11) . 2_676 ? C5 N1 C9 118.4(4) . . ? C5 N1 Cu1 122.2(3) . . ? C9 N1 Cu1 119.4(3) . . ? C3 O1 Cu1 107.0(2) . . ? C4 O3 Cu1 138.0(2) . 2_676 ? C4 O4 Cu1 138.2(3) . 1_565 ? C2 B3 C1 101.8(3) . . ? C2 B3 B7 106.2(3) . . ? C1 B3 B7 59.3(2) . . ? C2 B3 B11 59.5(3) . . ? C1 B3 B11 106.0(3) . . ? B7 B3 B11 60.9(3) . . ? C2 B3 B4 58.8(2) . . ? C1 B3 B4 58.6(2) . . ? B7 B3 B4 108.9(3) . . ? B11 B3 B4 109.1(3) . . ? C2 B3 H3 124.9 . . ? C1 B3 H3 125.2 . . ? B7 B3 H3 121.1 . . ? B11 B3 H3 121.1 . . ? B4 B3 H3 121.0 . . ? C2 B4 C1 101.7(3) . . ? C2 B4 B3 58.3(2) . . ? C1 B4 B3 59.0(2) . . ? C2 B4 B8 58.9(2) . . ? C1 B4 B8 104.6(3) . . ? B3 B4 B8 107.6(3) . . ? C2 B4 B5 105.0(3) . . ? C1 B4 B5 58.1(2) . . ? B3 B4 B5 107.5(3) . . ? B8 B4 B5 60.2(2) . . ? C2 B4 H4 125.1 . . ? C1 B4 H4 125.3 . . ? B3 B4 H4 121.6 . . ? B8 B4 H4 122.1 . . ? B5 B4 H4 122.3 . . ? C1 B5 B6 59.2(3) . . ? C1 B5 B8 104.5(3) . . ? B6 B5 B8 107.5(4) . . ? C1 B5 B4 58.5(2) . . ? B6 B5 B4 107.8(3) . . ? B8 B5 B4 59.7(2) . . ? C1 B5 B9 103.9(4) . . ? B6 B5 B9 58.7(3) . . ? B8 B5 B9 60.2(3) . . ? B4 B5 B9 107.2(3) . . ? C1 B5 H5 124.8 . . ? B6 B5 H5 121.7 . . ? B8 B5 H5 122.4 . . ? B4 B5 H5 121.8 . . ? B9 B5 H5 123.2 . . ? C1 B6 B9 105.3(4) . . ? C1 B6 B5 58.0(3) . . ? B9 B6 B5 61.7(3) . . ? C1 B6 B10 105.0(3) . . ? B9 B6 B10 60.2(4) . . ? B5 B6 B10 109.6(4) . . ? C1 B6 B7 58.9(3) . . ? B9 B6 B7 107.9(4) . . ? B5 B6 B7 108.0(3) . . ? B10 B6 B7 59.7(3) . . ? C1 B6 H6 124.9 . . ? B9 B6 H6 121.7 . . ? B5 B6 H6 120.6 . . ? B10 B6 H6 121.9 . . ? B7 B6 H6 121.8 . . ? C1 B7 B3 58.8(2) . . ? C1 B7 B10 105.3(4) . . ? B3 B7 B10 107.7(3) . . ? C1 B7 B6 58.8(3) . . ? B3 B7 B6 107.7(4) . . ? B10 B7 B6 60.2(3) . . ? C1 B7 B11 104.6(3) . . ? B3 B7 B11 59.6(2) . . ? B10 B7 B11 59.6(3) . . ? B6 B7 B11 107.4(4) . . ? C1 B7 H7 124.4 . . ? B3 B7 H7 121.7 . . ? B10 B7 H7 122.2 . . ? B6 B7 H7 121.7 . . ? B11 B7 H7 122.9 . . ? C2 B8 B4 58.3(2) . . ? C2 B8 B5 104.5(3) . . ? B4 B8 B5 60.2(3) . . ? C2 B8 B12 58.8(3) . . ? B4 B8 B12 107.5(3) . . ? B5 B8 B12 107.4(4) . . ? C2 B8 B9 103.5(4) . . ? B4 B8 B9 108.0(3) . . ? B5 B8 B9 60.7(3) . . ? B12 B8 B9 58.3(3) . . ? C2 B8 H8 125.2 . . ? B4 B8 H8 121.4 . . ? B5 B8 H8 122.1 . . ? B12 B8 H8 122.3 . . ? B9 B8 H8 123.0 . . ? B12 B9 B6 108.7(4) . . ? B12 B9 B10 60.8(4) . . ? B6 B9 B10 60.4(3) . . ? B12 B9 B8 60.5(3) . . ? B6 B9 B8 107.3(3) . . ? B10 B9 B8 108.8(4) . . ? B12 B9 B5 107.8(3) . . ? B6 B9 B5 59.6(3) . . ? B10 B9 B5 108.1(4) . . ? B8 B9 B5 59.1(3) . . ? B12 B9 H9 121.1 . . ? B6 B9 H9 121.8 . . ? B10 B9 H9 120.9 . . ? B8 B9 H9 121.9 . . ? B5 B9 H9 122.4 . . ? B11 B10 B7 60.7(3) . . ? B11 B10 B9 107.3(4) . . ? B7 B10 B9 107.7(4) . . ? B11 B10 B6 108.2(3) . . ? B7 B10 B6 60.2(3) . . ? B9 B10 B6 59.4(4) . . ? B11 B10 B12 59.7(3) . . ? B7 B10 B12 107.7(3) . . ? B9 B10 B12 59.0(3) . . ? B6 B10 B12 106.5(4) . . ? B11 B10 H10 121.5 . . ? B7 B10 H10 121.3 . . ? B9 B10 H10 122.5 . . ? B6 B10 H10 122.2 . . ? B12 B10 H10 122.7 . . ? C2 B11 B3 58.1(2) . . ? C2 B11 B12 59.1(3) . . ? B3 B11 B12 107.5(3) . . ? C2 B11 B10 105.6(4) . . ? B3 B11 B10 107.7(3) . . ? B12 B11 B10 60.5(3) . . ? C2 B11 B7 104.1(3) . . ? B3 B11 B7 59.5(2) . . ? B12 B11 B7 107.6(4) . . ? B10 B11 B7 59.7(3) . . ? C2 B11 H11 124.6 . . ? B3 B11 H11 122.1 . . ? B12 B11 H11 121.4 . . ? B10 B11 H11 121.9 . . ? B7 B11 H11 123.0 . . ? C2 B12 B9 105.4(3) . . ? C2 B12 B11 58.9(3) . . ? B9 B12 B11 108.4(4) . . ? C2 B12 B10 104.8(4) . . ? B9 B12 B10 60.3(4) . . ? B11 B12 B10 59.8(3) . . ? C2 B12 B8 58.3(2) . . ? B9 B12 B8 61.2(3) . . ? B11 B12 B8 108.2(3) . . ? B10 B12 B8 109.0(4) . . ? C2 B12 H12 124.8 . . ? B9 B12 H12 121.6 . . ? B11 B12 H12 121.5 . . ? B10 B12 H12 122.1 . . ? B8 B12 H12 120.9 . . ? C3 C1 B5 120.1(3) . . ? C3 C1 B4 119.7(3) . . ? B5 C1 B4 63.4(3) . . ? C3 C1 B3 117.0(3) . . ? B5 C1 B3 114.5(3) . . ? B4 C1 B3 62.4(2) . . ? C3 C1 B6 117.9(3) . . ? B5 C1 B6 62.7(3) . . ? B4 C1 B6 114.6(3) . . ? B3 C1 B6 113.1(3) . . ? C3 C1 B7 114.9(3) . . ? B5 C1 B7 114.9(3) . . ? B4 C1 B7 114.3(3) . . ? B3 C1 B7 61.9(2) . . ? B6 C1 B7 62.4(3) . . ? C4 C2 B3 117.9(3) . . ? C4 C2 B4 119.1(3) . . ? B3 C2 B4 62.9(2) . . ? C4 C2 B8 119.0(3) . . ? B3 C2 B8 114.4(3) . . ? B4 C2 B8 62.8(3) . . ? C4 C2 B11 116.0(3) . . ? B3 C2 B11 62.4(3) . . ? B4 C2 B11 114.9(3) . . ? B8 C2 B11 114.6(3) . . ? C4 C2 B12 117.5(3) . . ? B3 C2 B12 113.3(3) . . ? B4 C2 B12 114.6(3) . . ? B8 C2 B12 63.0(3) . . ? B11 C2 B12 62.0(3) . . ? O2 C3 O1 126.2(3) . . ? O2 C3 C1 119.0(3) . . ? O1 C3 C1 114.8(3) . . ? O3 C4 O4 128.9(3) . . ? O3 C4 C2 117.1(3) . . ? O4 C4 C2 114.0(3) . . ? N1 C5 C6 122.0(5) . . ? N1 C5 H5A 119.0 . . ? C6 C5 H5A 119.0 . . ? C7 C6 C5 119.2(5) . . ? C7 C6 H6A 120.4 . . ? C5 C6 H6A 120.4 . . ? C6 C7 C8 120.0(5) . . ? C6 C7 H7A 120.0 . . ? C8 C7 H7A 120.0 . . ? C9 C8 C7 118.2(5) . . ? C9 C8 H8A 120.9 . . ? C7 C8 H8A 120.9 . . ? N1 C9 C8 122.1(5) . . ? N1 C9 H9A 119.0 . . ? C8 C9 H9A 119.0 . . ? C10 N2 C14 120.0 . . ? C10 N2 Cu1 111.3(3) . . ? C14 N2 Cu1 128.3(3) . . ? C11 C10 N2 120.0 . . ? C11 C10 H10A 120.0 . . ? N2 C10 H10A 120.0 . . ? C10 C11 C12 120.0 . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C13 C12 C11 120.0 . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C14 C13 C12 120.0 . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 N2 120.0 . . ? C13 C14 H14 120.0 . . ? N2 C14 H14 120.0 . . ? C10' N2' C14' 120.0 . . ? C10' N2' Cu1 124.2(4) . . ? C14' N2' Cu1 115.7(4) . . ? C11' C10' N2' 120.0 . . ? C11' C10' H10' 120.0 . . ? N2' C10' H10' 120.0 . . ? C10' C11' C12' 120.0 . . ? C10' C11' H11' 120.0 . . ? C12' C11' H11' 120.0 . . ? C13' C12' C11' 120.0 . . ? C13' C12' H12' 120.0 . . ? C11' C12' H12' 120.0 . . ? C12' C13' C14' 120.0 . . ? C12' C13' H13' 120.0 . . ? C14' C13' H13' 120.0 . . ? C13' C14' N2' 120.0 . . ? C13' C14' H14' 120.0 . . ? N2' C14' H14' 120.0 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.546 _refine_diff_density_min -0.696 _refine_diff_density_rms 0.204 # Attachment '- 4th-revised Compound-5.cif' data_mo_00624a_0m _database_code_depnum_ccdc_archive 'CCDC 873638' #TrackingRef '- 4th-revised Compound-5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10.25 H29.25 B20 Cu2 N0.75 O10.75' _chemical_formula_weight 678.37 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' B B 0.0013 0.0007 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 12.037(4) _cell_length_b 18.567(6) _cell_length_c 17.116(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.077(5) _cell_angle_gamma 90.00 _cell_volume 3740(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2795 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 27.40 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 1.176 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9016 _exptl_absorpt_correction_T_max 0.9436 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23982 _diffrn_reflns_av_R_equivalents 0.1077 _diffrn_reflns_av_sigmaI/netI 0.1270 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6798 _reflns_number_gt 3154 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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. In this data, 7 DFIX and 5 ISOR instructions were used to refine disordered water molecule and DMF solvent molecule so that there were 37 restraints. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.031 0.250 -0.256 579.5 79.3 2 -0.010 0.750 0.256 579.1 77.1 3 0.233 0.750 0.745 25.0 3.1 4 0.766 0.250 0.255 24.7 1.0 _platon_squeeze_details ; ; _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^)+(0.1184P)^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 6798 _refine_ls_number_parameters 452 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.1436 _refine_ls_R_factor_gt 0.0750 _refine_ls_wR_factor_ref 0.2118 _refine_ls_wR_factor_gt 0.1861 _refine_ls_goodness_of_fit_ref 0.888 _refine_ls_restrained_S_all 0.895 _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 Cu1 Cu 0.47887(6) 0.53974(4) 0.06119(4) 0.0280(2) Uani 1 1 d . . . Cu2 Cu 1.09720(7) 0.46158(5) 0.51344(5) 0.0429(3) Uani 1 1 d . . . O1 O 0.6390(4) 0.5210(3) 0.1105(3) 0.0552(15) Uani 1 1 d U A . O2 O 0.6727(4) 0.4556(3) 0.0090(3) 0.0487(13) Uani 1 1 d . . . O3 O 1.0597(4) 0.4518(3) 0.3977(3) 0.0576(15) Uani 1 1 d . . . O4 O 0.8988(5) 0.5147(3) 0.3740(3) 0.0668(17) Uani 1 1 d U . . O5 O 0.4407(4) 0.4462(2) 0.1022(3) 0.0453(13) Uani 1 1 d . A . O6 O 0.4740(4) 0.3804(3) -0.0001(3) 0.0531(14) Uani 1 1 d . . . O7 O 1.1697(5) 0.5543(3) 0.5008(4) 0.0652(17) Uani 1 1 d . . . O8 O 1.0084(5) 0.6192(3) 0.4807(4) 0.0726(18) Uani 1 1 d . . . O10 O 1.2431(5) 0.3970(4) 0.5304(4) 0.116(3) Uani 1 1 d . . . H10A H 1.2281 0.3728 0.4881 0.140 Uiso 1 1 d R . . H10B H 1.2690 0.3700 0.5685 0.140 Uiso 1 1 d R . . B1 B 0.3711(10) 0.2500 0.0445(8) 0.045(3) Uani 1 2 d S . . H1 H 0.3572 0.2500 -0.0223 0.054 Uiso 1 2 calc SR . . B2 B 0.5099(10) 0.2500 0.1077(7) 0.036(3) Uani 1 2 d S . . H2 H 0.5874 0.2500 0.0811 0.043 Uiso 1 2 calc SR . . B3 B 0.2780(13) 0.2500 0.1904(9) 0.059(4) Uani 1 2 d S . . H3 H 0.2013 0.2500 0.2178 0.071 Uiso 1 2 calc SR . . B4 B 0.5071(8) 0.2971(5) 0.1964(5) 0.051(2) Uani 1 1 d . . . H4 H 0.5816 0.3298 0.2273 0.061 Uiso 1 1 calc R . . B5 B 0.3627(8) 0.3239(6) 0.1924(6) 0.058(3) Uani 1 1 d . . . H5 H 0.3415 0.3744 0.2219 0.069 Uiso 1 1 calc R . . B6 B 0.4190(12) 0.2500 0.2502(8) 0.050(4) Uani 1 2 d S . . H6 H 0.4374 0.2500 0.3171 0.059 Uiso 1 2 calc SR . . B7 B 0.2812(7) 0.2984(5) 0.0993(6) 0.053(3) Uani 1 1 d . . . H7 H 0.2079 0.3315 0.0671 0.064 Uiso 1 1 calc R . . B8 B 1.0468(7) 0.4575(5) 0.1286(5) 0.047(2) Uani 1 1 d . . . H8 H 1.1202 0.4658 0.0988 0.057 Uiso 1 1 calc R . . B9 B 0.8452(7) 0.3755(5) 0.1402(5) 0.044(2) Uani 1 1 d . . . H9 H 0.7850 0.3305 0.1177 0.053 Uiso 1 1 calc R . . B10 B 0.9434(7) 0.3733(5) 0.2367(5) 0.046(2) Uani 1 1 d . . . H10 H 0.9497 0.3266 0.2789 0.055 Uiso 1 1 calc R . . B11 B 0.9306(7) 0.5173(5) 0.1126(5) 0.043(2) Uani 1 1 d . . . H11 H 0.9257 0.5650 0.0720 0.052 Uiso 1 1 calc R . . B12 B 1.0244(8) 0.5141(5) 0.2069(5) 0.045(2) Uani 1 1 d . . . H12 H 1.0838 0.5593 0.2301 0.054 Uiso 1 1 calc R . . B13 B 0.9959(7) 0.3695(5) 0.1462(5) 0.044(2) Uani 1 1 d . . . H13 H 1.0356 0.3195 0.1278 0.053 Uiso 1 1 calc R . . B14 B 1.0639(8) 0.4230(5) 0.2286(5) 0.049(2) Uani 1 1 d . . . H14 H 1.1489 0.4084 0.2659 0.059 Uiso 1 1 calc R . . B15 B 0.9135(7) 0.4272(5) 0.0747(5) 0.045(2) Uani 1 1 d . . . H15 H 0.8978 0.4157 0.0091 0.054 Uiso 1 1 calc R . . B16 B 0.8235(7) 0.4335(5) 0.2179(5) 0.039(2) Uani 1 1 d . . . H16 H 0.7494 0.4262 0.2473 0.047 Uiso 1 1 calc R . . B17 B 0.8738(7) 0.5205(4) 0.2001(5) 0.042(2) Uani 1 1 d . . . H17 H 0.8323 0.5704 0.2173 0.050 Uiso 1 1 calc R . . B18 B 1.3311(15) 0.7500 0.4106(11) 0.081(5) Uani 1 2 d S . . H18 H 1.3886 0.7500 0.3668 0.098 Uiso 1 2 calc SR . . B19 B 1.2023(10) 0.7009(7) 0.3915(6) 0.081(4) Uani 1 1 d . . . H19 H 1.1743 0.6675 0.3364 0.097 Uiso 1 1 calc R . . B20 B 1.1060(12) 0.7500 0.4348(7) 0.050(3) Uani 1 2 d S . . H20 H 1.0131 0.7500 0.4068 0.060 Uiso 1 2 calc SR . . B21 B 1.1571(13) 0.7500 0.5414(8) 0.058(4) Uani 1 2 d S . . H21 H 1.0974 0.7500 0.5835 0.069 Uiso 1 2 calc SR . . B22 B 1.2849(9) 0.7035(6) 0.5622(7) 0.077(3) Uani 1 1 d . . . H22 H 1.3114 0.6716 0.6186 0.092 Uiso 1 1 calc R . . B23 B 1.3144(9) 0.6737(6) 0.4701(7) 0.074(3) Uani 1 1 d . . . H23 H 1.3617 0.6224 0.4659 0.088 Uiso 1 1 calc R . . B24 B 1.3806(15) 0.7500 0.5187(11) 0.095(6) Uani 1 2 d S . . H24 H 1.4734 0.7500 0.5467 0.113 Uiso 1 2 calc SR . . C1 C 0.9649(6) 0.4733(3) 0.3542(3) 0.0320(17) Uani 1 1 d U . . C2 C 0.6934(5) 0.4762(3) 0.0826(4) 0.0275(15) Uani 1 1 d U . . C3 C 0.4492(6) 0.3883(4) 0.0673(4) 0.0322(16) Uani 1 1 d . . . C4 C 1.1144(8) 0.6118(5) 0.4892(5) 0.059(2) Uani 1 1 d . . . C5 C 0.9558(6) 0.4620(4) 0.2649(4) 0.0391(17) Uani 1 1 d . . . C6 C 0.8161(6) 0.4643(4) 0.1248(4) 0.0360(16) Uani 1 1 d . A . C7 C 0.4195(6) 0.3214(3) 0.1061(4) 0.0328(16) Uani 1 1 d . A . C8 C 1.1797(7) 0.6786(4) 0.4842(4) 0.050(2) Uani 1 1 d . . . C9 C 0.3700(18) 0.4607(10) 0.3984(12) 0.145(8) Uani 0.75 1 d PDU . . H9E H 0.2914 0.4711 0.3812 0.174 Uiso 0.75 1 calc PR . . C10 C 0.3821(15) 0.5435(6) 0.2906(8) 0.118(7) Uani 0.75 1 d PD . . H10C H 0.3941 0.5926 0.3116 0.177 Uiso 0.75 1 calc PR . . H10D H 0.3004 0.5337 0.2752 0.177 Uiso 0.75 1 calc PR . . H10E H 0.4164 0.5385 0.2437 0.177 Uiso 0.75 1 calc PR . . C11 C 0.5553(15) 0.4876(14) 0.3534(14) 0.218(13) Uani 0.75 1 d PD . . H11A H 0.5691 0.4973 0.3000 0.328 Uiso 0.75 1 calc PR . . H11B H 0.5824 0.4391 0.3703 0.328 Uiso 0.75 1 calc PR . . H11C H 0.5961 0.5230 0.3913 0.328 Uiso 0.75 1 calc PR . . O11 O 0.3907(14) 0.4203(9) 0.4599(10) 0.199(7) Uani 0.75 1 d PD . . N1 N 0.4345(14) 0.4924(8) 0.3517(8) 0.125(5) Uani 0.75 1 d PDU . . O9 O 0.4212(13) 0.6205(8) 0.1324(8) 0.071(5) Uani 0.50 1 d PU A 1 H9A H 0.3861 0.5894 0.1551 0.106 Uiso 0.50 1 d PR A 1 H9B H 0.4761 0.6338 0.1695 0.106 Uiso 0.50 1 d PR A 1 O9' O 0.4563(14) 0.5899(9) 0.1675(9) 0.090(6) Uani 0.50 1 d PU A 2 H9C H 0.3846 0.5897 0.1533 0.134 Uiso 0.50 1 d PR A 2 H9D H 0.4747 0.6340 0.1676 0.134 Uiso 0.50 1 d PR A 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 Cu1 0.0299(5) 0.0278(4) 0.0245(4) -0.0046(4) 0.0018(3) 0.0031(4) Cu2 0.0350(5) 0.0572(6) 0.0320(5) -0.0092(5) -0.0034(4) 0.0099(5) O1 0.041(3) 0.072(4) 0.046(3) -0.009(3) -0.007(3) 0.010(3) O2 0.037(3) 0.063(3) 0.042(3) -0.006(3) -0.001(2) 0.013(3) O3 0.053(4) 0.072(4) 0.046(3) -0.010(3) 0.006(3) 0.006(3) O4 0.058(4) 0.101(5) 0.034(3) -0.009(3) -0.005(3) 0.020(3) O5 0.060(3) 0.030(3) 0.045(3) 0.009(2) 0.011(3) -0.002(2) O6 0.067(4) 0.033(3) 0.062(4) 0.004(3) 0.021(3) -0.004(3) O7 0.054(4) 0.056(4) 0.083(4) 0.003(3) 0.008(3) 0.002(3) O8 0.069(4) 0.063(4) 0.088(5) -0.007(4) 0.022(4) 0.000(4) O10 0.080(5) 0.151(7) 0.120(6) 0.034(5) 0.026(5) 0.067(5) B1 0.037(7) 0.031(7) 0.064(9) 0.000 0.002(7) 0.000 B2 0.032(7) 0.032(6) 0.040(7) 0.000 0.001(6) 0.000 B3 0.065(10) 0.047(8) 0.079(10) 0.000 0.049(9) 0.000 B4 0.055(6) 0.047(6) 0.044(5) -0.005(4) -0.003(5) 0.008(5) B5 0.062(7) 0.063(7) 0.053(6) -0.007(5) 0.025(5) 0.006(5) B6 0.084(11) 0.028(7) 0.042(7) 0.000 0.024(7) 0.000 B7 0.030(5) 0.053(6) 0.078(7) -0.013(5) 0.015(5) -0.008(4) B8 0.033(5) 0.061(6) 0.043(5) 0.004(5) -0.002(4) 0.001(5) B9 0.037(5) 0.057(6) 0.037(5) -0.003(4) 0.003(4) 0.002(4) B10 0.034(5) 0.051(6) 0.051(5) -0.002(5) 0.006(4) 0.007(4) B11 0.036(5) 0.043(5) 0.047(5) 0.008(4) 0.000(4) -0.011(4) B12 0.041(5) 0.053(6) 0.037(5) -0.007(4) 0.004(4) -0.004(4) B13 0.036(5) 0.048(5) 0.052(5) -0.006(5) 0.014(4) 0.007(4) B14 0.039(5) 0.060(6) 0.046(5) 0.000(5) 0.001(4) 0.015(5) B15 0.042(5) 0.053(5) 0.041(5) -0.012(4) 0.013(4) 0.006(5) B16 0.041(5) 0.046(5) 0.031(5) 0.003(4) 0.009(4) -0.005(4) B17 0.036(5) 0.042(5) 0.041(5) -0.007(4) -0.007(4) 0.006(4) B18 0.080(13) 0.071(11) 0.100(14) 0.000 0.032(11) 0.000 B19 0.098(10) 0.110(9) 0.038(6) -0.011(6) 0.022(6) -0.004(8) B20 0.059(9) 0.059(9) 0.027(6) 0.000 -0.005(6) 0.000 B21 0.077(11) 0.048(8) 0.037(7) 0.000 -0.013(7) 0.000 B22 0.071(8) 0.074(7) 0.071(7) 0.010(6) -0.018(6) 0.002(6) B23 0.052(7) 0.072(8) 0.096(9) 0.008(7) 0.015(7) 0.000(6) B24 0.062(12) 0.124(16) 0.091(14) 0.000 0.001(10) 0.000 C1 0.038(4) 0.039(4) 0.015(3) -0.009(3) -0.004(3) 0.019(3) C2 0.027(2) 0.027(2) 0.025(2) -0.0092(17) -0.0011(17) 0.0103(17) C3 0.038(4) 0.021(4) 0.036(4) 0.003(3) 0.004(3) -0.002(3) C4 0.062(6) 0.075(7) 0.037(5) -0.005(5) 0.004(5) 0.001(6) C5 0.029(4) 0.053(4) 0.033(4) -0.006(4) 0.001(3) 0.001(4) C6 0.034(4) 0.044(4) 0.029(3) -0.005(3) 0.003(3) -0.006(3) C7 0.036(4) 0.030(4) 0.033(4) 0.001(3) 0.007(3) 0.006(3) C8 0.056(5) 0.050(5) 0.044(5) -0.011(4) 0.007(4) -0.003(4) C9 0.153(15) 0.140(14) 0.135(14) 0.002(12) 0.013(13) 0.004(13) C10 0.23(2) 0.045(8) 0.063(9) -0.012(7) -0.006(11) -0.030(10) C11 0.15(2) 0.27(3) 0.26(3) -0.05(2) 0.07(2) 0.05(2) O11 0.214(17) 0.206(16) 0.181(15) 0.052(13) 0.050(13) 0.051(13) N1 0.170(13) 0.125(11) 0.092(9) -0.010(8) 0.056(10) -0.014(10) O9 0.081(8) 0.084(8) 0.055(7) -0.041(6) 0.033(6) -0.012(7) O9' 0.079(10) 0.112(12) 0.081(11) -0.043(9) 0.026(9) 0.002(9) _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 O5 1.963(4) . ? Cu1 O2 1.965(5) 3_665 ? Cu1 O6 1.965(5) 3_665 ? Cu1 O1 1.967(5) . ? Cu1 O9' 2.111(15) . ? Cu1 O9 2.137(14) . ? Cu1 Cu1 2.6962(16) 3_665 ? Cu2 O3 1.946(5) . ? Cu2 O7 1.963(6) . ? Cu2 O4 1.967(5) 3_766 ? Cu2 O8 1.982(6) 3_766 ? Cu2 O10 2.095(6) . ? Cu2 Cu2 2.6967(18) 3_766 ? O1 C2 1.216(7) . ? O2 C2 1.289(7) . ? O2 Cu1 1.965(5) 3_665 ? O3 C1 1.288(8) . ? O4 C1 1.204(7) . ? O4 Cu2 1.967(5) 3_766 ? O5 C3 1.244(7) . ? O6 C3 1.258(8) . ? O6 Cu1 1.965(5) 3_665 ? O7 C4 1.251(10) . ? O8 C4 1.261(10) . ? O8 Cu2 1.982(6) 3_766 ? B1 C7 1.718(10) . ? B1 C7 1.718(10) 4_565 ? B1 B2 1.790(16) . ? B1 B7 1.812(14) . ? B1 B7 1.812(14) 4_565 ? B2 C7 1.711(9) 4_565 ? B2 C7 1.711(9) . ? B2 B4 1.759(13) . ? B2 B4 1.759(13) 4_565 ? B3 B5 1.706(13) . ? B3 B5 1.706(13) 4_565 ? B3 B6 1.79(2) . ? B3 B7 1.807(15) 4_565 ? B3 B7 1.807(15) . ? B4 C7 1.738(11) . ? B4 B4 1.750(18) 4_565 ? B4 B6 1.774(14) . ? B4 B5 1.795(13) . ? B5 B6 1.744(13) . ? B5 B7 1.753(13) . ? B5 C7 1.753(11) . ? B6 B5 1.744(13) 4_565 ? B6 B4 1.774(14) 4_565 ? B7 C7 1.699(10) . ? B7 B7 1.799(18) 4_565 ? B8 B11 1.762(12) . ? B8 B12 1.767(12) . ? B8 B15 1.767(12) . ? B8 B13 1.793(12) . ? B8 B14 1.799(12) . ? B9 C6 1.695(11) . ? B9 B16 1.773(11) . ? B9 B13 1.799(11) . ? B9 B15 1.800(12) . ? B9 B10 1.820(12) . ? B10 C5 1.714(11) . ? B10 B14 1.749(13) . ? B10 B13 1.792(12) . ? B10 B16 1.802(12) . ? B11 C6 1.741(10) . ? B11 B12 1.768(12) . ? B11 B17 1.772(12) . ? B11 B15 1.790(12) . ? B12 C5 1.716(11) . ? B12 B14 1.774(13) . ? B12 B17 1.796(12) . ? B13 B15 1.767(12) . ? B13 B14 1.779(12) . ? B14 C5 1.714(11) . ? B15 C6 1.732(10) . ? B16 C6 1.677(10) . ? B16 C5 1.711(10) . ? B16 B17 1.774(12) . ? B17 C6 1.690(10) . ? B17 C5 1.711(10) . ? B18 B19 1.769(18) . ? B18 B19 1.769(18) 4_575 ? B18 B23 1.782(15) . ? B18 B23 1.782(15) 4_575 ? B18 B24 1.82(2) . ? B19 C8 1.716(12) . ? B19 B20 1.756(16) . ? B19 B23 1.769(15) . ? B19 B19 1.82(2) 4_575 ? B20 C8 1.716(11) 4_575 ? B20 C8 1.716(11) . ? B20 B19 1.756(16) 4_575 ? B20 B21 1.800(17) . ? B21 C8 1.703(11) 4_575 ? B21 C8 1.703(11) . ? B21 B22 1.735(16) 4_575 ? B21 B22 1.735(16) . ? B22 C8 1.701(13) . ? B22 B22 1.73(2) 4_575 ? B22 B24 1.729(18) . ? B22 B23 1.775(15) . ? B23 C8 1.690(13) . ? B23 B24 1.748(15) . ? B24 B22 1.729(18) 4_575 ? B24 B23 1.748(15) 4_575 ? C1 C5 1.524(8) . ? C2 C6 1.518(9) . ? C3 C7 1.487(8) . ? C4 C8 1.481(11) . ? C9 O11 1.275(15) . ? C9 N1 1.360(15) . ? C10 N1 1.454(14) . ? C11 N1 1.450(15) . ? 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 O5 Cu1 O2 90.1(2) . 3_665 ? O5 Cu1 O6 166.6(2) . 3_665 ? O2 Cu1 O6 88.6(2) 3_665 3_665 ? O5 Cu1 O1 88.4(2) . . ? O2 Cu1 O1 166.2(2) 3_665 . ? O6 Cu1 O1 89.7(2) 3_665 . ? O5 Cu1 O9' 90.0(5) . . ? O2 Cu1 O9' 103.7(5) 3_665 . ? O6 Cu1 O9' 103.3(5) 3_665 . ? O1 Cu1 O9' 90.0(5) . . ? O5 Cu1 O9 106.8(4) . . ? O2 Cu1 O9 86.9(4) 3_665 . ? O6 Cu1 O9 86.5(4) 3_665 . ? O1 Cu1 O9 106.6(4) . . ? O9' Cu1 O9 23.6(5) . . ? O5 Cu1 Cu1 83.67(15) . 3_665 ? O2 Cu1 Cu1 81.45(14) 3_665 3_665 ? O6 Cu1 Cu1 82.91(15) 3_665 3_665 ? O1 Cu1 Cu1 84.76(15) . 3_665 ? O9' Cu1 Cu1 171.9(5) . 3_665 ? O9 Cu1 Cu1 164.4(4) . 3_665 ? O3 Cu2 O7 89.1(2) . . ? O3 Cu2 O4 166.1(2) . 3_766 ? O7 Cu2 O4 89.5(3) . 3_766 ? O3 Cu2 O8 88.0(2) . 3_766 ? O7 Cu2 O8 166.9(2) . 3_766 ? O4 Cu2 O8 90.3(2) 3_766 3_766 ? O3 Cu2 O10 95.5(3) . . ? O7 Cu2 O10 97.9(3) . . ? O4 Cu2 O10 98.3(3) 3_766 . ? O8 Cu2 O10 95.0(3) 3_766 . ? O3 Cu2 Cu2 82.39(16) . 3_766 ? O7 Cu2 Cu2 84.66(18) . 3_766 ? O4 Cu2 Cu2 83.73(17) 3_766 3_766 ? O8 Cu2 Cu2 82.31(19) 3_766 3_766 ? O10 Cu2 Cu2 176.7(2) . 3_766 ? C2 O1 Cu1 120.8(4) . . ? C2 O2 Cu1 123.3(4) . 3_665 ? C1 O3 Cu2 123.2(4) . . ? C1 O4 Cu2 122.5(5) . 3_766 ? C3 O5 Cu1 123.0(4) . . ? C3 O6 Cu1 123.4(4) . 3_665 ? C4 O7 Cu2 122.1(6) . . ? C4 O8 Cu2 123.7(6) . 3_766 ? C7 B1 C7 101.0(8) . 4_565 ? C7 B1 B2 58.3(5) . . ? C7 B1 B2 58.3(5) 4_565 . ? C7 B1 B7 57.5(5) . . ? C7 B1 B7 103.2(8) 4_565 . ? B2 B1 B7 105.7(8) . . ? C7 B1 B7 103.2(8) . 4_565 ? C7 B1 B7 57.5(5) 4_565 4_565 ? B2 B1 B7 105.7(8) . 4_565 ? B7 B1 B7 59.5(7) . 4_565 ? C7 B2 C7 101.5(7) 4_565 . ? C7 B2 B4 105.8(7) 4_565 . ? C7 B2 B4 60.1(4) . . ? C7 B2 B4 60.1(4) 4_565 4_565 ? C7 B2 B4 105.8(7) . 4_565 ? B4 B2 B4 59.7(7) . 4_565 ? C7 B2 B1 58.7(4) 4_565 . ? C7 B2 B1 58.7(4) . . ? B4 B2 B1 109.7(7) . . ? B4 B2 B1 109.7(7) 4_565 . ? B5 B3 B5 107.1(10) . 4_565 ? B5 B3 B6 59.8(6) . . ? B5 B3 B6 59.8(6) 4_565 . ? B5 B3 B7 107.3(8) . 4_565 ? B5 B3 B7 59.8(5) 4_565 4_565 ? B6 B3 B7 107.8(7) . 4_565 ? B5 B3 B7 59.8(5) . . ? B5 B3 B7 107.3(8) 4_565 . ? B6 B3 B7 107.8(8) . . ? B7 B3 B7 59.7(7) 4_565 . ? C7 B4 B4 105.0(4) . 4_565 ? C7 B4 B2 58.6(4) . . ? B4 B4 B2 60.2(3) 4_565 . ? C7 B4 B6 105.8(7) . . ? B4 B4 B6 60.5(4) 4_565 . ? B2 B4 B6 108.9(7) . . ? C7 B4 B5 59.5(5) . . ? B4 B4 B5 106.1(4) 4_565 . ? B2 B4 B5 107.3(7) . . ? B6 B4 B5 58.5(6) . . ? B3 B5 B6 62.5(7) . . ? B3 B5 B7 63.0(7) . . ? B6 B5 B7 112.4(7) . . ? B3 B5 C7 107.4(7) . . ? B6 B5 C7 106.5(7) . . ? B7 B5 C7 58.0(5) . . ? B3 B5 B4 110.4(7) . . ? B6 B5 B4 60.2(6) . . ? B7 B5 B4 108.3(6) . . ? C7 B5 B4 58.6(4) . . ? B5 B6 B5 103.8(10) 4_565 . ? B5 B6 B4 61.4(5) 4_565 4_565 ? B5 B6 B4 107.3(8) . 4_565 ? B5 B6 B4 107.3(8) 4_565 . ? B5 B6 B4 61.4(5) . . ? B4 B6 B4 59.1(7) 4_565 . ? B5 B6 B3 57.7(5) 4_565 . ? B5 B6 B3 57.7(5) . . ? B4 B6 B3 107.5(8) 4_565 . ? B4 B6 B3 107.5(8) . . ? C7 B7 B5 61.0(5) . . ? C7 B7 B7 104.5(4) . 4_565 ? B5 B7 B7 105.6(5) . 4_565 ? C7 B7 B3 105.3(7) . . ? B5 B7 B3 57.2(6) . . ? B7 B7 B3 60.2(4) 4_565 . ? C7 B7 B1 58.5(5) . . ? B5 B7 B1 108.8(7) . . ? B7 B7 B1 60.2(4) 4_565 . ? B3 B7 B1 108.8(7) . . ? B11 B8 B12 60.1(5) . . ? B11 B8 B15 61.0(5) . . ? B12 B8 B15 108.6(6) . . ? B11 B8 B13 108.2(6) . . ? B12 B8 B13 107.6(6) . . ? B15 B8 B13 59.5(5) . . ? B11 B8 B14 107.6(6) . . ? B12 B8 B14 59.7(5) . . ? B15 B8 B14 107.1(6) . . ? B13 B8 B14 59.4(5) . . ? C6 B9 B16 57.8(4) . . ? C6 B9 B13 104.0(6) . . ? B16 B9 B13 107.4(6) . . ? C6 B9 B15 59.3(5) . . ? B16 B9 B15 107.5(6) . . ? B13 B9 B15 58.8(5) . . ? C6 B9 B10 103.7(6) . . ? B16 B9 B10 60.2(5) . . ? B13 B9 B10 59.4(5) . . ? B15 B9 B10 106.4(6) . . ? C5 B10 B14 59.3(5) . . ? C5 B10 B13 104.8(6) . . ? B14 B10 B13 60.3(5) . . ? C5 B10 B16 58.2(4) . . ? B14 B10 B16 107.7(6) . . ? B13 B10 B16 106.5(6) . . ? C5 B10 B9 103.6(6) . . ? B14 B10 B9 108.0(6) . . ? B13 B10 B9 59.7(5) . . ? B16 B10 B9 58.6(4) . . ? C6 B11 B8 104.3(6) . . ? C6 B11 B12 104.0(6) . . ? B8 B11 B12 60.1(5) . . ? C6 B11 B17 57.5(4) . . ? B8 B11 B17 108.9(6) . . ? B12 B11 B17 61.0(5) . . ? C6 B11 B15 58.7(4) . . ? B8 B11 B15 59.7(5) . . ? B12 B11 B15 107.6(6) . . ? B17 B11 B15 107.5(6) . . ? C5 B12 B8 105.7(6) . . ? C5 B12 B11 104.7(6) . . ? B8 B12 B11 59.8(5) . . ? C5 B12 B14 58.8(5) . . ? B8 B12 B14 61.0(5) . . ? B11 B12 B14 108.4(6) . . ? C5 B12 B17 58.3(4) . . ? B8 B12 B17 107.5(6) . . ? B11 B12 B17 59.6(5) . . ? B14 B12 B17 107.4(6) . . ? B15 B13 B14 108.0(6) . . ? B15 B13 B10 109.1(6) . . ? B14 B13 B10 58.7(5) . . ? B15 B13 B8 59.5(5) . . ? B14 B13 B8 60.5(5) . . ? B10 B13 B8 107.7(6) . . ? B15 B13 B9 60.6(5) . . ? B14 B13 B9 107.6(6) . . ? B10 B13 B9 60.9(5) . . ? B8 B13 B9 108.1(6) . . ? C5 B14 B10 59.3(5) . . ? C5 B14 B12 58.9(5) . . ? B10 B14 B12 109.3(6) . . ? C5 B14 B13 105.3(6) . . ? B10 B14 B13 61.0(5) . . ? B12 B14 B13 107.9(6) . . ? C5 B14 B8 104.5(6) . . ? B10 B14 B8 109.4(6) . . ? B12 B14 B8 59.3(5) . . ? B13 B14 B8 60.2(5) . . ? C6 B15 B13 103.8(6) . . ? C6 B15 B8 104.5(6) . . ? B13 B15 B8 61.0(5) . . ? C6 B15 B11 59.2(4) . . ? B13 B15 B11 108.1(6) . . ? B8 B15 B11 59.4(5) . . ? C6 B15 B9 57.3(4) . . ? B13 B15 B9 60.6(5) . . ? B8 B15 B9 109.2(6) . . ? B11 B15 B9 107.9(6) . . ? C6 B16 C5 101.6(5) . . ? C6 B16 B9 58.8(4) . . ? C5 B16 B9 105.8(6) . . ? C6 B16 B17 58.6(4) . . ? C5 B16 B17 58.8(4) . . ? B9 B16 B17 108.4(6) . . ? C6 B16 B10 105.2(6) . . ? C5 B16 B10 58.3(4) . . ? B9 B16 B10 61.2(5) . . ? B17 B16 B10 107.9(6) . . ? C6 B17 C5 101.0(5) . . ? C6 B17 B11 60.3(4) . . ? C5 B17 B11 104.7(6) . . ? C6 B17 B16 57.9(4) . . ? C5 B17 B16 58.8(4) . . ? B11 B17 B16 108.7(6) . . ? C6 B17 B12 104.9(6) . . ? C5 B17 B12 58.5(4) . . ? B11 B17 B12 59.4(5) . . ? B16 B17 B12 107.7(6) . . ? B19 B18 B19 62.0(10) . 4_575 ? B19 B18 B23 59.7(6) . . ? B19 B18 B23 108.4(10) 4_575 . ? B19 B18 B23 108.4(10) . 4_575 ? B19 B18 B23 59.7(6) 4_575 4_575 ? B23 B18 B23 105.4(12) . 4_575 ? B19 B18 B24 106.0(10) . . ? B19 B18 B24 106.0(10) 4_575 . ? B23 B18 B24 58.0(7) . . ? B23 B18 B24 58.0(7) 4_575 . ? C8 B19 B20 59.2(5) . . ? C8 B19 B23 58.0(6) . . ? B20 B19 B23 107.0(8) . . ? C8 B19 B18 104.8(9) . . ? B20 B19 B18 106.6(8) . . ? B23 B19 B18 60.5(7) . . ? C8 B19 B19 104.0(5) . 4_575 ? B20 B19 B19 58.7(5) . 4_575 ? B23 B19 B19 106.6(6) . 4_575 ? B18 B19 B19 59.0(5) . 4_575 ? C8 B20 C8 101.1(8) 4_575 . ? C8 B20 B19 59.2(5) 4_575 4_575 ? C8 B20 B19 106.8(9) . 4_575 ? C8 B20 B19 106.8(9) 4_575 . ? C8 B20 B19 59.2(5) . . ? B19 B20 B19 62.5(9) 4_575 . ? C8 B20 B21 57.9(5) 4_575 . ? C8 B20 B21 57.9(5) . . ? B19 B20 B21 108.2(9) 4_575 . ? B19 B20 B21 108.2(9) . . ? C8 B21 C8 102.1(9) 4_575 . ? C8 B21 B22 59.3(6) 4_575 4_575 ? C8 B21 B22 105.3(10) . 4_575 ? C8 B21 B22 105.3(10) 4_575 . ? C8 B21 B22 59.3(6) . . ? B22 B21 B22 59.8(9) 4_575 . ? C8 B21 B20 58.6(5) 4_575 . ? C8 B21 B20 58.6(5) . . ? B22 B21 B20 108.0(9) 4_575 . ? B22 B21 B20 108.0(9) . . ? C8 B22 B22 105.7(5) . 4_575 ? C8 B22 B24 104.5(9) . . ? B22 B22 B24 60.0(5) 4_575 . ? C8 B22 B21 59.4(5) . . ? B22 B22 B21 60.1(4) 4_575 . ? B24 B22 B21 107.7(9) . . ? C8 B22 B23 58.1(5) . . ? B22 B22 B23 108.2(5) 4_575 . ? B24 B22 B23 59.8(7) . . ? B21 B22 B23 107.8(8) . . ? C8 B23 B24 104.1(9) . . ? C8 B23 B19 59.4(5) . . ? B24 B23 B19 109.2(9) . . ? C8 B23 B22 58.7(6) . . ? B24 B23 B22 58.8(8) . . ? B19 B23 B22 108.9(8) . . ? C8 B23 B18 105.4(9) . . ? B24 B23 B18 62.1(8) . . ? B19 B23 B18 59.8(8) . . ? B22 B23 B18 109.1(9) . . ? B22 B24 B22 60.0(10) . 4_575 ? B22 B24 B23 61.4(7) . . ? B22 B24 B23 109.4(11) 4_575 . ? B22 B24 B23 109.4(11) . 4_575 ? B22 B24 B23 61.4(7) 4_575 4_575 ? B23 B24 B23 108.3(12) . 4_575 ? B22 B24 B18 109.4(11) . . ? B22 B24 B18 109.4(11) 4_575 . ? B23 B24 B18 59.9(7) . . ? B23 B24 B18 59.9(7) 4_575 . ? O4 C1 O3 126.3(6) . . ? O4 C1 C5 117.2(6) . . ? O3 C1 C5 113.9(6) . . ? O1 C2 O2 125.2(6) . . ? O1 C2 C6 117.5(6) . . ? O2 C2 C6 113.1(5) . . ? O5 C3 O6 126.8(6) . . ? O5 C3 C7 117.2(6) . . ? O6 C3 C7 115.9(6) . . ? O7 C4 O8 127.1(9) . . ? O7 C4 C8 116.9(8) . . ? O8 C4 C8 116.0(8) . . ? C1 C5 B16 112.2(5) . . ? C1 C5 B17 118.2(6) . . ? B16 C5 B17 62.4(5) . . ? C1 C5 B10 113.5(6) . . ? B16 C5 B10 63.5(5) . . ? B17 C5 B10 115.1(5) . . ? C1 C5 B14 121.4(6) . . ? B16 C5 B14 113.7(6) . . ? B17 C5 B14 114.3(6) . . ? B10 C5 B14 61.4(5) . . ? C1 C5 B12 124.0(6) . . ? B16 C5 B12 114.6(5) . . ? B17 C5 B12 63.2(5) . . ? B10 C5 B12 113.8(6) . . ? B14 C5 B12 62.3(5) . . ? C2 C6 B16 110.8(5) . . ? C2 C6 B17 118.4(6) . . ? B16 C6 B17 63.6(5) . . ? C2 C6 B9 111.4(5) . . ? B16 C6 B9 63.4(5) . . ? B17 C6 B9 116.4(6) . . ? C2 C6 B15 120.9(5) . . ? B16 C6 B15 115.3(6) . . ? B17 C6 B15 114.2(6) . . ? B9 C6 B15 63.3(5) . . ? C2 C6 B11 125.1(6) . . ? B16 C6 B11 114.9(6) . . ? B17 C6 B11 62.2(5) . . ? B9 C6 B11 115.2(6) . . ? B15 C6 B11 62.0(5) . . ? C3 C7 B7 120.2(6) . . ? C3 C7 B2 116.3(6) . . ? B7 C7 B2 114.7(6) . . ? C3 C7 B1 117.0(6) . . ? B7 C7 B1 64.1(6) . . ? B2 C7 B1 63.0(5) . . ? C3 C7 B4 117.1(6) . . ? B7 C7 B4 113.5(6) . . ? B2 C7 B4 61.3(5) . . ? B1 C7 B4 114.3(6) . . ? C3 C7 B5 121.7(6) . . ? B7 C7 B5 61.0(5) . . ? B2 C7 B5 111.5(6) . . ? B1 C7 B5 113.3(7) . . ? B4 C7 B5 61.9(5) . . ? C4 C8 B23 119.9(7) . . ? C4 C8 B22 119.9(7) . . ? B23 C8 B22 63.1(6) . . ? C4 C8 B21 117.9(7) . . ? B23 C8 B21 113.4(8) . . ? B22 C8 B21 61.3(6) . . ? C4 C8 B19 116.4(7) . . ? B23 C8 B19 62.6(6) . . ? B22 C8 B19 115.2(7) . . ? B21 C8 B19 114.8(7) . . ? C4 C8 B20 116.7(7) . . ? B23 C8 B20 112.6(8) . . ? B22 C8 B20 113.6(7) . . ? B21 C8 B20 63.5(6) . . ? B19 C8 B20 61.6(6) . . ? O11 C9 N1 135(2) . . ? C9 N1 C11 130.8(18) . . ? C9 N1 C10 119.3(17) . . ? C11 N1 C10 109.8(13) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.489 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.135 # Attachment '- 3_rev_Compound-6.cif' data_mo_10503ba _database_code_depnum_ccdc_archive 'CCDC 873639' #TrackingRef '- 3_rev_Compound-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12.75 H39 B20 Cu2 O12.75' _chemical_formula_weight 739.72 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' O O 0.0106 0.0060 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' 'x-1/2, y, -z-1/2' _cell_length_a 21.0039(14) _cell_length_b 18.1673(12) _cell_length_c 18.7689(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7161.9(8) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9877 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 28.27 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3004 _exptl_absorpt_coefficient_mu 1.237 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5546 _exptl_absorpt_correction_T_max 0.8080 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEX-II CCD' _diffrn_measurement_method ' \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54304 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 28.28 _reflns_number_total 9124 _reflns_number_gt 7074 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0768P)^2^+19.4720P] 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 9124 _refine_ls_number_parameters 480 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0644 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1571 _refine_ls_wR_factor_gt 0.1384 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.002 _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 Cu1 Cu 0.540090(16) 0.956905(18) 0.464152(17) 0.01506(10) Uani 1 1 d . . . Cu2 Cu 0.453046(16) 0.958140(18) 0.975791(18) 0.01577(10) Uani 1 1 d . . . O1 O 0.58585(11) 0.95156(14) 0.55530(12) 0.0301(5) Uani 1 1 d . . . O2 O 0.51820(12) 1.02341(14) 0.61577(12) 0.0301(5) Uani 1 1 d . . . O3 O 0.50802(11) 0.95172(14) 0.89146(12) 0.0309(5) Uani 1 1 d . . . O4 O 0.58813(11) 1.02113(14) 0.93220(12) 0.0306(5) Uani 1 1 d . . . O5 O 0.48324(11) 0.88012(12) 0.49982(13) 0.0297(5) Uani 1 1 d . . . O6 O 0.41517(11) 0.95171(12) 0.56039(13) 0.0274(5) Uani 1 1 d . . . O7 O 0.50379(11) 0.88121(12) 1.02103(14) 0.0310(5) Uani 1 1 d . . . O8 O 0.58387(12) 0.95068(12) 1.06156(14) 0.0299(5) Uani 1 1 d . . . O9 O 0.59915(13) 0.88562(14) 0.40207(13) 0.0358(6) Uani 1 1 d . . . H9' H 0.6256 0.8671 0.4291 0.054 Uiso 1 1 d R . . O10 O 0.37965(12) 0.88869(14) 0.93368(13) 0.0333(5) Uiso 1 1 d . . . H10D H 0.3450 0.8952 0.9562 0.050 Uiso 1 1 d R . . B1 B 0.55658(17) 0.93358(18) 0.74822(17) 0.0206(6) Uani 1 1 d . . . H1 H 0.5038 0.9250 0.7470 0.025 Uiso 1 1 calc R . . B2 B 0.59053(17) 1.0240(2) 0.74972(17) 0.0216(6) Uani 1 1 d . . . H2 H 0.5601 1.0746 0.7497 0.026 Uiso 1 1 calc R . . B3 B 0.66398(18) 1.0206(2) 0.7033(2) 0.0284(8) Uani 1 1 d . . . H3 H 0.6819 1.0686 0.6716 0.034 Uiso 1 1 calc R . . B4 B 0.67594(17) 0.9275(2) 0.6747(2) 0.0296(8) Uani 1 1 d . . . H4 H 0.7020 0.9146 0.6242 0.035 Uiso 1 1 calc R . . B5 B 0.60936(18) 0.8742(2) 0.70187(19) 0.0261(7) Uani 1 1 d . . . H5 H 0.5917 0.8268 0.6693 0.031 Uiso 1 1 calc R . . B6 B 0.66267(17) 1.0203(2) 0.79797(19) 0.0266(7) Uani 1 1 d . . . H6 H 0.6799 1.0681 0.8304 0.032 Uiso 1 1 calc R . . B7 B 0.71543(18) 0.9608(3) 0.7515(2) 0.0347(9) Uani 1 1 d . . . H7 H 0.7682 0.9697 0.7526 0.042 Uiso 1 1 calc R . . B8 B 0.6817(2) 0.8705(3) 0.7508(2) 0.0344(9) Uani 1 1 d . . . H8 H 0.7121 0.8198 0.7516 0.041 Uiso 1 1 calc R . . B9 B 0.60748(19) 0.8742(2) 0.79610(19) 0.0270(7) Uani 1 1 d . . . H9 H 0.5884 0.8266 0.8274 0.032 Uiso 1 1 calc R . . B10 B 0.67323(18) 0.9274(2) 0.82665(19) 0.0304(8) Uani 1 1 d . . . H10 H 0.6975 0.9144 0.8783 0.037 Uiso 1 1 calc R . . B11 B 0.33040(17) 0.7989(2) 0.53217(19) 0.0241(7) Uani 1 1 d . . . H11 H 0.3036 0.8319 0.4917 0.029 Uiso 1 1 calc R . . B12 B 0.33824(16) 0.82896(19) 0.62255(19) 0.0234(7) Uani 1 1 d . . . H12 H 0.3164 0.8818 0.6411 0.028 Uiso 1 1 calc R . . B13 B 0.41404(16) 0.79927(19) 0.65526(18) 0.0218(6) Uani 1 1 d . . . H13 H 0.4416 0.8325 0.6949 0.026 Uiso 1 1 calc R . . B14 B 0.4521(2) 0.7500 0.5857(3) 0.0196(9) Uani 1 2 d S . . H14 H 0.5051 0.7500 0.5798 0.024 Uiso 1 2 calc SR . . B15 B 0.4009(2) 0.7500 0.5101(3) 0.0199(9) Uani 1 2 d S . . H15 H 0.4205 0.7500 0.4547 0.024 Uiso 1 2 calc SR . . B16 B 0.2915(2) 0.7500 0.6024(3) 0.0261(10) Uani 1 2 d S . . H16 H 0.2384 0.7500 0.6081 0.031 Uiso 1 2 calc SR . . B17 B 0.3430(2) 0.7500 0.6783(3) 0.0250(10) Uani 1 2 d S . . H17 H 0.3238 0.7500 0.7340 0.030 Uiso 1 2 calc SR . . B18 B 0.57694(18) 0.7989(2) 1.16799(18) 0.0250(7) Uani 1 1 d . . . H18 H 0.5491 0.8320 1.2075 0.030 Uiso 1 1 calc R . . B19 B 0.65259(18) 0.8287(2) 1.1361(2) 0.0268(7) Uani 1 1 d . . . H19 H 0.6743 0.8816 1.1548 0.032 Uiso 1 1 calc R . . B20 B 0.66123(17) 0.7985(2) 1.0465(2) 0.0245(7) Uani 1 1 d . . . H20 H 0.6885 0.8316 1.0063 0.029 Uiso 1 1 calc R . . B21 B 0.5914(2) 0.7500 1.0230(3) 0.0202(9) Uani 1 2 d S . . H21 H 0.5726 0.7500 0.9671 0.024 Uiso 1 2 calc SR . . B22 B 0.5389(2) 0.7500 1.0981(3) 0.0213(9) Uani 1 2 d S . . H22 H 0.4859 0.7500 1.0916 0.026 Uiso 1 2 calc SR . . B23 B 0.6472(3) 0.7500 1.1918(3) 0.0302(11) Uani 1 2 d S . . H23 H 0.6657 0.7500 1.2477 0.036 Uiso 1 2 calc SR . . B24 B 0.6995(3) 0.7500 1.1164(3) 0.0297(11) Uani 1 2 d S . . H24 H 0.7525 0.7500 1.1226 0.036 Uiso 1 2 calc SR . . C1 C 0.60094(14) 0.96553(17) 0.67929(15) 0.0196(6) Uani 1 1 d . . . C2 C 0.56541(14) 0.98227(17) 0.61048(15) 0.0213(6) Uani 1 1 d . . . C3 C 0.59872(14) 0.96514(16) 0.81931(15) 0.0198(6) Uani 1 1 d . . . C4 C 0.56165(14) 0.98132(17) 0.88712(15) 0.0201(6) Uani 1 1 d . . . C5 C 0.40351(13) 0.82209(15) 0.56723(16) 0.0188(5) Uani 1 1 d . . . C6 C 0.43649(15) 0.89111(16) 0.53984(15) 0.0202(6) Uani 1 1 d . . . C7 C 0.58809(14) 0.82199(16) 1.08030(15) 0.0194(6) Uani 1 1 d . . . C8 C 0.55566(14) 0.89122(16) 1.05189(16) 0.0203(6) Uani 1 1 d . . . C9 C 0.6284(2) 0.9135(3) 0.3388(2) 0.0502(11) Uani 1 1 d . . . H9A H 0.5953 0.9286 0.3049 0.075 Uiso 1 1 calc R . . H9B H 0.6548 0.8750 0.3172 0.075 Uiso 1 1 calc R . . H9C H 0.6550 0.9560 0.3508 0.075 Uiso 1 1 calc R . . C10 C 0.3596(2) 0.9039(4) 0.8596(3) 0.0687(15) Uani 1 1 d . . . H10A H 0.3392 0.9523 0.8573 0.103 Uiso 1 1 calc R . . H10B H 0.3295 0.8661 0.8439 0.103 Uiso 1 1 calc R . . H10C H 0.3970 0.9035 0.8283 0.103 Uiso 1 1 calc R . . C11 C 0.5237(5) 0.2500 0.6739(5) 0.094(3) Uani 1 2 d S . . H11A H 0.5433 0.2987 0.6690 0.141 Uiso 0.50 1 calc PR . . H11B H 0.5511 0.2130 0.6515 0.141 Uiso 0.50 1 calc PR . . H11C H 0.5184 0.2383 0.7245 0.141 Uiso 0.50 1 calc PR . . C12 C 0.2549(2) 0.0169(4) 0.5098(3) 0.084(2) Uani 1 1 d . . . H12A H 0.2681 0.0064 0.5588 0.125 Uiso 1 1 calc R . . H12B H 0.2913 0.0110 0.4777 0.125 Uiso 1 1 calc R . . H12C H 0.2210 -0.0173 0.4958 0.125 Uiso 1 1 calc R . . C13 C 0.3409(5) 0.2500 0.4706(5) 0.094(3) Uani 1 2 d S . . H13A H 0.3475 0.2990 0.4911 0.141 Uiso 0.50 1 calc PR . . H13B H 0.3105 0.2533 0.4312 0.141 Uiso 0.50 1 calc PR . . H13C H 0.3816 0.2309 0.4529 0.141 Uiso 0.50 1 calc PR . . C14 C 0.0402(6) 0.2500 0.3623(8) 0.125(5) Uani 1 2 d S . . H14A H 0.0021 0.2226 0.3765 0.188 Uiso 0.50 1 calc PR . . H14B H 0.0594 0.2265 0.3204 0.188 Uiso 0.50 1 calc PR . . H14C H 0.0285 0.3008 0.3506 0.188 Uiso 0.50 1 calc PR . . O11 O 0.4618(3) 0.2500 0.6390(4) 0.089(2) Uani 1 2 d S . . H11D H 0.4588 0.2129 0.6126 0.133 Uiso 0.50 1 calc PR . . O12 O 0.2322(2) 0.0892(3) 0.5055(2) 0.0939(14) Uani 1 1 d . . . H12D H 0.2328 0.1038 0.5507 0.141 Uiso 1 1 d R . . O13 O 0.3145(3) 0.1977(4) 0.5284(4) 0.0606(18) Uani 0.50 1 d P . . H13D H 0.2881 0.1630 0.5212 0.091 Uiso 0.50 1 d PR . . O14 O 0.0836(4) 0.2500 0.4178(5) 0.124(3) Uani 1 2 d S . . H14D H 0.0956 0.2056 0.4224 0.187 Uiso 0.50 1 d PR . . O15 O 0.2412(5) 0.2078(5) 0.6016(5) 0.035(2) Uiso 0.25 1 d P . . H15A H 0.2657 0.1971 0.6342 0.042 Uiso 0.25 1 d PR . . C15 C 0.1800(11) 0.2500 0.6169(14) 0.118(8) Uiso 0.50 2 d SP . . H15B H 0.1432 0.2195 0.6040 0.178 Uiso 0.25 1 calc PR . . H15C H 0.1794 0.2954 0.5887 0.178 Uiso 0.25 1 calc PR . . H15D H 0.1780 0.2622 0.6677 0.178 Uiso 0.25 1 calc PR . . 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 0.01825(18) 0.01489(18) 0.01206(17) 0.00050(12) 0.00109(12) 0.00145(12) Cu2 0.01815(18) 0.01517(18) 0.01399(17) -0.00098(12) -0.00174(12) 0.00001(12) O1 0.0303(12) 0.0456(15) 0.0143(10) -0.0022(10) -0.0036(9) 0.0115(10) O2 0.0330(12) 0.0402(13) 0.0170(10) -0.0026(10) -0.0060(9) 0.0115(11) O3 0.0269(12) 0.0447(14) 0.0213(11) -0.0097(10) 0.0046(9) -0.0070(10) O4 0.0305(12) 0.0412(14) 0.0200(11) -0.0099(10) 0.0049(9) -0.0074(10) O5 0.0347(13) 0.0173(10) 0.0372(13) 0.0001(9) 0.0160(10) -0.0025(9) O6 0.0281(11) 0.0177(10) 0.0364(13) -0.0002(9) 0.0117(10) -0.0007(9) O7 0.0312(12) 0.0190(11) 0.0429(14) 0.0035(10) -0.0139(11) 0.0003(9) O8 0.0328(12) 0.0157(10) 0.0413(14) 0.0019(9) -0.0143(11) -0.0002(9) O9 0.0425(14) 0.0360(14) 0.0288(12) -0.0015(10) 0.0094(11) 0.0151(11) B1 0.0245(15) 0.0212(15) 0.0159(14) -0.0001(12) -0.0010(12) -0.0024(13) B2 0.0261(16) 0.0229(15) 0.0159(14) 0.0000(12) -0.0010(12) -0.0013(13) B3 0.0266(17) 0.038(2) 0.0203(16) -0.0001(15) -0.0003(13) -0.0075(15) B4 0.0230(17) 0.045(2) 0.0210(17) -0.0022(15) -0.0011(13) 0.0076(16) B5 0.0348(19) 0.0256(17) 0.0179(15) -0.0015(13) 0.0009(14) 0.0074(15) B6 0.0244(17) 0.036(2) 0.0192(16) -0.0026(14) -0.0013(13) -0.0089(15) B7 0.0210(16) 0.063(3) 0.0207(17) -0.0035(18) -0.0010(13) 0.0028(17) B8 0.035(2) 0.046(2) 0.0217(17) -0.0014(16) -0.0028(15) 0.0216(18) B9 0.039(2) 0.0231(17) 0.0187(16) 0.0007(13) 0.0008(14) 0.0073(15) B10 0.0261(17) 0.046(2) 0.0193(16) -0.0005(15) -0.0027(13) 0.0116(16) B11 0.0210(15) 0.0226(16) 0.0288(17) 0.0016(13) -0.0020(13) 0.0012(13) B12 0.0223(16) 0.0199(16) 0.0279(17) -0.0002(13) 0.0065(13) 0.0012(13) B13 0.0264(16) 0.0182(15) 0.0210(15) -0.0007(12) 0.0007(13) 0.0003(13) B14 0.019(2) 0.015(2) 0.025(2) 0.000 0.0012(17) 0.000 B15 0.024(2) 0.014(2) 0.021(2) 0.000 -0.0022(18) 0.000 B16 0.020(2) 0.022(2) 0.036(3) 0.000 0.004(2) 0.000 B17 0.027(2) 0.022(2) 0.026(2) 0.000 0.0088(19) 0.000 B18 0.0385(19) 0.0195(15) 0.0169(15) -0.0003(12) -0.0017(14) -0.0016(14) B19 0.0319(18) 0.0193(16) 0.0290(18) -0.0005(14) -0.0128(15) -0.0008(14) B20 0.0226(16) 0.0197(15) 0.0311(18) -0.0002(14) -0.0006(13) -0.0007(13) B21 0.025(2) 0.016(2) 0.019(2) 0.000 -0.0004(17) 0.000 B22 0.026(2) 0.018(2) 0.020(2) 0.000 0.0033(18) 0.000 B23 0.042(3) 0.020(2) 0.028(3) 0.000 -0.015(2) 0.000 B24 0.028(3) 0.020(2) 0.041(3) 0.000 -0.011(2) 0.000 C1 0.0197(13) 0.0251(14) 0.0140(13) 0.0013(11) -0.0023(10) 0.0016(11) C2 0.0230(14) 0.0259(15) 0.0150(13) 0.0035(11) -0.0021(11) -0.0026(12) C3 0.0223(13) 0.0239(14) 0.0133(12) -0.0007(11) -0.0010(10) 0.0018(11) C4 0.0224(14) 0.0234(14) 0.0145(12) 0.0019(11) 0.0000(10) 0.0042(11) C5 0.0196(13) 0.0149(12) 0.0218(14) 0.0002(10) 0.0021(11) -0.0001(10) C6 0.0239(14) 0.0183(14) 0.0186(13) 0.0026(11) -0.0006(11) -0.0023(11) C7 0.0237(14) 0.0152(12) 0.0192(13) -0.0006(10) -0.0013(11) -0.0004(11) C8 0.0242(14) 0.0183(14) 0.0184(13) 0.0024(11) 0.0009(11) 0.0022(11) C9 0.064(3) 0.052(3) 0.035(2) -0.0099(19) 0.024(2) 0.001(2) C10 0.056(3) 0.097(4) 0.053(3) -0.011(3) -0.020(2) -0.020(3) C11 0.092(7) 0.126(9) 0.064(6) 0.000 0.023(5) 0.000 C12 0.049(3) 0.110(5) 0.092(4) 0.062(4) 0.020(3) 0.015(3) C13 0.112(8) 0.109(8) 0.060(5) 0.000 0.029(5) 0.000 C14 0.095(9) 0.131(11) 0.150(12) 0.000 -0.034(8) 0.000 O11 0.094(5) 0.057(4) 0.115(6) 0.000 0.010(4) 0.000 O12 0.079(3) 0.116(4) 0.087(3) 0.007(3) -0.005(2) -0.016(3) O13 0.053(4) 0.050(4) 0.079(5) -0.004(3) 0.005(3) 0.002(3) O14 0.167(8) 0.061(4) 0.145(7) 0.000 -0.065(6) 0.000 _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 O5 1.954(2) . ? Cu1 O6 1.962(2) 5_676 ? Cu1 O1 1.965(2) . ? Cu1 O2 1.969(2) 5_676 ? Cu1 O9 2.139(2) . ? Cu1 Cu1 2.6644(7) 5_676 ? Cu2 O7 1.952(2) . ? Cu2 O8 1.959(2) 5_677 ? Cu2 O3 1.963(2) . ? Cu2 O4 1.968(2) 5_677 ? Cu2 O10 2.143(3) . ? Cu2 Cu2 2.6514(7) 5_677 ? O1 C2 1.252(4) . ? O2 C2 1.246(4) . ? O2 Cu1 1.969(2) 5_676 ? O3 C4 1.251(4) . ? O4 C4 1.244(4) . ? O4 Cu2 1.968(2) 5_677 ? O5 C6 1.252(4) . ? O6 C6 1.250(4) . ? O6 Cu1 1.962(2) 5_676 ? O7 C8 1.247(4) . ? O8 C8 1.245(4) . ? O8 Cu2 1.959(2) 5_677 ? O9 C9 1.430(5) . ? O9 H9' 0.8244 . ? O10 C10 1.480(5) . ? O10 H10D 0.8495 . ? B1 C1 1.697(4) . ? B1 C3 1.701(4) . ? B1 B9 1.764(5) . ? B1 B5 1.774(5) . ? B1 B2 1.790(5) . ? B1 H1 1.1200 . ? B2 C3 1.696(4) . ? B2 C1 1.709(4) . ? B2 B6 1.766(5) . ? B2 B3 1.773(5) . ? B2 H2 1.1200 . ? B3 C1 1.720(5) . ? B3 B6 1.777(5) . ? B3 B7 1.781(6) . ? B3 B4 1.793(6) . ? B3 H3 1.1200 . ? B4 C1 1.723(5) . ? B4 B8 1.768(6) . ? B4 B7 1.770(5) . ? B4 B5 1.775(6) . ? B4 H4 1.1200 . ? B5 C1 1.721(5) . ? B5 B9 1.769(5) . ? B5 B8 1.777(5) . ? B5 H5 1.1200 . ? B6 C3 1.723(5) . ? B6 B7 1.777(6) . ? B6 B10 1.786(6) . ? B6 H6 1.1200 . ? B7 B10 1.772(6) . ? B7 B8 1.787(7) . ? B7 H7 1.1200 . ? B8 B10 1.769(6) . ? B8 B9 1.777(6) . ? B8 H8 1.1200 . ? B9 C3 1.718(5) . ? B9 B10 1.780(6) . ? B9 H9 1.1200 . ? B10 C3 1.714(5) . ? B10 H10 1.1200 . ? B11 C5 1.723(5) . ? B11 B15 1.776(6) . ? B11 B11 1.777(7) 7_575 ? B11 B16 1.787(6) . ? B11 B12 1.790(5) . ? B11 H11 1.1200 . ? B12 C5 1.724(4) . ? B12 B17 1.779(5) . ? B12 B16 1.780(5) . ? B12 B13 1.789(5) . ? B12 H12 1.1200 . ? B13 C5 1.718(4) . ? B13 B14 1.773(5) . ? B13 B13 1.790(7) 7_575 ? B13 B17 1.793(6) . ? B13 H13 1.1200 . ? B14 C5 1.696(4) 7_575 ? B14 C5 1.696(4) . ? B14 B13 1.773(5) 7_575 ? B14 B15 1.779(7) . ? B14 H14 1.1200 . ? B15 C5 1.693(4) . ? B15 C5 1.693(4) 7_575 ? B15 B11 1.776(6) 7_575 ? B15 H15 1.1200 . ? B16 B12 1.780(5) 7_575 ? B16 B11 1.787(6) 7_575 ? B16 B17 1.790(8) . ? B16 H16 1.1200 . ? B17 B12 1.779(5) 7_575 ? B17 B13 1.793(6) 7_575 ? B17 H17 1.1200 . ? B18 C7 1.715(4) . ? B18 B22 1.774(6) . ? B18 B18 1.776(7) 7_575 ? B18 B23 1.779(6) . ? B18 B19 1.782(5) . ? B18 H18 1.1200 . ? B19 C7 1.716(5) . ? B19 B23 1.775(5) . ? B19 B24 1.775(5) . ? B19 B20 1.778(5) . ? B19 H19 1.1200 . ? B20 C7 1.716(5) . ? B20 B20 1.764(7) 7_575 ? B20 B21 1.768(6) . ? B20 B24 1.774(6) . ? B20 H20 1.1200 . ? B21 C7 1.695(4) . ? B21 C7 1.695(4) 7_575 ? B21 B20 1.768(6) 7_575 ? B21 B22 1.790(7) . ? B21 H21 1.1200 . ? B22 C7 1.700(4) 7_575 ? B22 C7 1.700(4) . ? B22 B18 1.774(6) 7_575 ? B22 H22 1.1200 . ? B23 B19 1.775(5) 7_575 ? B23 B18 1.779(6) 7_575 ? B23 B24 1.792(9) . ? B23 H23 1.1200 . ? B24 B20 1.774(6) 7_575 ? B24 B19 1.775(5) 7_575 ? B24 H24 1.1200 . ? C1 C2 1.522(4) . ? C3 C4 1.521(4) . ? C5 C6 1.522(4) . ? C7 C8 1.527(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 O11 1.455(12) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 O12 1.400(8) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 O13 1.545(9) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 O14 1.385(13) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? O11 H11D 0.8400 . ? O12 H12D 0.8879 . ? O13 H13D 0.8503 . ? O14 H14D 0.8494 . ? O15 C15 1.52(2) . ? O15 H15A 0.8236 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C15 H15D 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 O5 Cu1 O6 167.61(9) . 5_676 ? O5 Cu1 O1 88.01(11) . . ? O6 Cu1 O1 90.69(11) 5_676 . ? O5 Cu1 O2 90.61(11) . 5_676 ? O6 Cu1 O2 88.01(11) 5_676 5_676 ? O1 Cu1 O2 167.57(10) . 5_676 ? O5 Cu1 O9 96.25(10) . . ? O6 Cu1 O9 96.12(10) 5_676 . ? O1 Cu1 O9 99.25(10) . . ? O2 Cu1 O9 93.19(10) 5_676 . ? O5 Cu1 Cu1 81.97(7) . 5_676 ? O6 Cu1 Cu1 85.64(7) 5_676 5_676 ? O1 Cu1 Cu1 84.17(7) . 5_676 ? O2 Cu1 Cu1 83.40(7) 5_676 5_676 ? O9 Cu1 Cu1 176.11(8) . 5_676 ? O7 Cu2 O8 167.78(10) . 5_677 ? O7 Cu2 O3 89.26(11) . . ? O8 Cu2 O3 89.69(11) 5_677 . ? O7 Cu2 O4 89.72(11) . 5_677 ? O8 Cu2 O4 88.76(11) 5_677 5_677 ? O3 Cu2 O4 167.87(10) . 5_677 ? O7 Cu2 O10 97.57(10) . . ? O8 Cu2 O10 94.65(9) 5_677 . ? O3 Cu2 O10 95.21(10) . . ? O4 Cu2 O10 96.90(10) 5_677 . ? O7 Cu2 Cu2 81.69(7) . 5_677 ? O8 Cu2 Cu2 86.10(7) 5_677 5_677 ? O3 Cu2 Cu2 82.69(7) . 5_677 ? O4 Cu2 Cu2 85.20(7) 5_677 5_677 ? O10 Cu2 Cu2 177.77(7) . 5_677 ? C2 O1 Cu1 122.0(2) . . ? C2 O2 Cu1 122.9(2) . 5_676 ? C4 O3 Cu2 123.8(2) . . ? C4 O4 Cu2 120.8(2) . 5_677 ? C6 O5 Cu1 124.8(2) . . ? C6 O6 Cu1 120.1(2) . 5_676 ? C8 O7 Cu2 125.1(2) . . ? C8 O8 Cu2 119.5(2) . 5_677 ? C9 O9 Cu1 119.2(2) . . ? C9 O9 H9' 111.5 . . ? Cu1 O9 H9' 107.6 . . ? C10 O10 Cu2 116.2(3) . . ? C10 O10 H10D 101.5 . . ? Cu2 O10 H10D 110.5 . . ? C1 B1 C3 101.4(2) . . ? C1 B1 B9 105.4(2) . . ? C3 B1 B9 59.41(19) . . ? C1 B1 B5 59.39(19) . . ? C3 B1 B5 105.3(2) . . ? B9 B1 B5 60.0(2) . . ? C1 B1 B2 58.64(18) . . ? C3 B1 B2 58.07(18) . . ? B9 B1 B2 108.1(2) . . ? B5 B1 B2 108.4(2) . . ? C1 B1 H1 125.1 . . ? C3 B1 H1 125.3 . . ? B9 B1 H1 121.7 . . ? B5 B1 H1 121.6 . . ? B2 B1 H1 121.4 . . ? C3 B2 C1 101.0(2) . . ? C3 B2 B6 59.65(19) . . ? C1 B2 B6 105.3(2) . . ? C3 B2 B3 105.6(2) . . ? C1 B2 B3 59.16(19) . . ? B6 B2 B3 60.3(2) . . ? C3 B2 B1 58.32(18) . . ? C1 B2 B1 57.94(18) . . ? B6 B2 B1 108.4(3) . . ? B3 B2 B1 107.9(3) . . ? C3 B2 H2 125.1 . . ? C1 B2 H2 125.6 . . ? B6 B2 H2 121.4 . . ? B3 B2 H2 121.7 . . ? B1 B2 H2 121.7 . . ? C1 B3 B2 58.58(19) . . ? C1 B3 B6 104.4(2) . . ? B2 B3 B6 59.7(2) . . ? C1 B3 B7 104.2(3) . . ? B2 B3 B7 107.4(3) . . ? B6 B3 B7 59.9(2) . . ? C1 B3 B4 58.7(2) . . ? B2 B3 B4 107.5(3) . . ? B6 B3 B4 107.4(3) . . ? B7 B3 B4 59.4(2) . . ? C1 B3 H3 124.9 . . ? B2 B3 H3 121.8 . . ? B6 B3 H3 122.6 . . ? B7 B3 H3 122.8 . . ? B4 B3 H3 121.9 . . ? C1 B4 B8 104.9(3) . . ? C1 B4 B7 104.5(3) . . ? B8 B4 B7 60.7(2) . . ? C1 B4 B5 58.92(19) . . ? B8 B4 B5 60.2(2) . . ? B7 B4 B5 108.7(3) . . ? C1 B4 B3 58.5(2) . . ? B8 B4 B3 108.7(3) . . ? B7 B4 B3 60.0(2) . . ? B5 B4 B3 108.5(3) . . ? C1 B4 H4 125.0 . . ? B8 B4 H4 121.9 . . ? B7 B4 H4 122.1 . . ? B5 B4 H4 121.0 . . ? B3 B4 H4 121.2 . . ? C1 B5 B9 104.1(2) . . ? C1 B5 B1 58.06(18) . . ? B9 B5 B1 59.7(2) . . ? C1 B5 B4 59.0(2) . . ? B9 B5 B4 107.7(3) . . ? B1 B5 B4 107.6(3) . . ? C1 B5 B8 104.6(3) . . ? B9 B5 B8 60.2(2) . . ? B1 B5 B8 107.7(3) . . ? B4 B5 B8 59.7(2) . . ? C1 B5 H5 125.0 . . ? B9 B5 H5 122.6 . . ? B1 B5 H5 121.9 . . ? B4 B5 H5 121.6 . . ? B8 B5 H5 122.4 . . ? C3 B6 B2 58.15(18) . . ? C3 B6 B3 104.2(2) . . ? B2 B6 B3 60.0(2) . . ? C3 B6 B7 104.2(3) . . ? B2 B6 B7 107.8(3) . . ? B3 B6 B7 60.1(2) . . ? C3 B6 B10 58.4(2) . . ? B2 B6 B10 107.2(3) . . ? B3 B6 B10 107.6(3) . . ? B7 B6 B10 59.6(2) . . ? C3 B6 H6 125.2 . . ? B2 B6 H6 121.8 . . ? B3 B6 H6 122.4 . . ? B7 B6 H6 122.5 . . ? B10 B6 H6 121.9 . . ? B4 B7 B10 107.3(3) . . ? B4 B7 B6 108.4(3) . . ? B10 B7 B6 60.4(2) . . ? B4 B7 B3 60.7(2) . . ? B10 B7 B3 108.1(3) . . ? B6 B7 B3 59.9(2) . . ? B4 B7 B8 59.6(2) . . ? B10 B7 B8 59.6(2) . . ? B6 B7 B8 108.4(3) . . ? B3 B7 B8 108.4(3) . . ? B4 B7 H7 121.8 . . ? B10 B7 H7 122.1 . . ? B6 B7 H7 121.3 . . ? B3 B7 H7 121.3 . . ? B8 B7 H7 121.7 . . ? B4 B8 B10 107.5(3) . . ? B4 B8 B5 60.1(2) . . ? B10 B8 B5 107.9(3) . . ? B4 B8 B9 107.7(3) . . ? B10 B8 B9 60.3(2) . . ? B5 B8 B9 59.7(2) . . ? B4 B8 B7 59.7(2) . . ? B10 B8 B7 59.8(2) . . ? B5 B8 B7 107.9(3) . . ? B9 B8 B7 108.0(3) . . ? B4 B8 H8 122.0 . . ? B10 B8 H8 121.8 . . ? B5 B8 H8 121.8 . . ? B9 B8 H8 121.7 . . ? B7 B8 H8 121.8 . . ? C3 B9 B1 58.45(18) . . ? C3 B9 B5 104.8(2) . . ? B1 B9 B5 60.3(2) . . ? C3 B9 B8 104.6(3) . . ? B1 B9 B8 108.1(3) . . ? B5 B9 B8 60.1(2) . . ? C3 B9 B10 58.6(2) . . ? B1 B9 B10 107.6(3) . . ? B5 B9 B10 107.7(3) . . ? B8 B9 B10 59.6(2) . . ? C3 B9 H9 124.8 . . ? B1 B9 H9 121.5 . . ? B5 B9 H9 122.2 . . ? B8 B9 H9 122.4 . . ? B10 B9 H9 121.8 . . ? C3 B10 B8 105.1(3) . . ? C3 B10 B7 104.8(3) . . ? B8 B10 B7 60.6(2) . . ? C3 B10 B9 58.9(2) . . ? B8 B10 B9 60.1(2) . . ? B7 B10 B9 108.5(3) . . ? C3 B10 B6 58.9(2) . . ? B8 B10 B6 108.8(3) . . ? B7 B10 B6 59.9(2) . . ? B9 B10 B6 108.6(2) . . ? C3 B10 H10 124.7 . . ? B8 B10 H10 121.8 . . ? B7 B10 H10 122.2 . . ? B9 B10 H10 121.2 . . ? B6 B10 H10 121.1 . . ? C5 B11 B15 57.86(19) . . ? C5 B11 B11 104.15(15) . 7_575 ? B15 B11 B11 59.97(14) . 7_575 ? C5 B11 B16 104.4(3) . . ? B15 B11 B16 107.7(2) . . ? B11 B11 B16 60.18(15) 7_575 . ? C5 B11 B12 58.76(19) . . ? B15 B11 B12 107.3(3) . . ? B11 B11 B12 107.76(16) 7_575 . ? B16 B11 B12 59.7(2) . . ? C5 B11 H11 125.2 . . ? B15 B11 H11 122.0 . . ? B11 B11 H11 122.4 7_575 . ? B16 B11 H11 122.4 . . ? B12 B11 H11 121.7 . . ? C5 B12 B17 104.5(3) . . ? C5 B12 B16 104.6(3) . . ? B17 B12 B16 60.4(2) . . ? C5 B12 B13 58.49(18) . . ? B17 B12 B13 60.3(2) . . ? B16 B12 B13 108.7(3) . . ? C5 B12 B11 58.68(19) . . ? B17 B12 B11 108.5(3) . . ? B16 B12 B11 60.1(2) . . ? B13 B12 B11 108.4(2) . . ? C5 B12 H12 125.1 . . ? B17 B12 H12 122.1 . . ? B16 B12 H12 122.0 . . ? B13 B12 H12 121.1 . . ? B11 B12 H12 121.2 . . ? C5 B13 B14 58.10(19) . . ? C5 B13 B12 58.85(18) . . ? B14 B13 B12 107.5(3) . . ? C5 B13 B13 103.96(15) . 7_575 ? B14 B13 B13 59.68(13) . 7_575 ? B12 B13 B13 107.54(16) . 7_575 ? C5 B13 B17 104.2(3) . . ? B14 B13 B17 107.5(2) . . ? B12 B13 B17 59.5(2) . . ? B13 B13 B17 60.04(14) 7_575 . ? C5 B13 H13 125.1 . . ? B14 B13 H13 121.9 . . ? B12 B13 H13 121.7 . . ? B13 B13 H13 122.7 7_575 . ? B17 B13 H13 122.6 . . ? C5 B14 C5 101.1(3) 7_575 . ? C5 B14 B13 59.31(18) 7_575 7_575 ? C5 B14 B13 105.6(3) . 7_575 ? C5 B14 B13 105.6(3) 7_575 . ? C5 B14 B13 59.31(18) . . ? B13 B14 B13 60.6(3) 7_575 . ? C5 B14 B15 58.26(19) 7_575 . ? C5 B14 B15 58.26(19) . . ? B13 B14 B15 108.3(3) 7_575 . ? B13 B14 B15 108.3(3) . . ? C5 B14 H14 125.3 7_575 . ? C5 B14 H14 125.3 . . ? B13 B14 H14 121.4 7_575 . ? B13 B14 H14 121.4 . . ? B15 B14 H14 121.5 . . ? C5 B15 C5 101.4(3) . 7_575 ? C5 B15 B11 105.5(3) . 7_575 ? C5 B15 B11 59.50(19) 7_575 7_575 ? C5 B15 B11 59.50(19) . . ? C5 B15 B11 105.5(3) 7_575 . ? B11 B15 B11 60.1(3) 7_575 . ? C5 B15 B14 58.41(18) . . ? C5 B15 B14 58.41(18) 7_575 . ? B11 B15 B14 108.6(3) 7_575 . ? B11 B15 B14 108.6(3) . . ? C5 B15 H15 125.2 . . ? C5 B15 H15 125.2 7_575 . ? B11 B15 H15 121.5 7_575 . ? B11 B15 H15 121.5 . . ? B14 B15 H15 121.3 . . ? B12 B16 B12 107.4(4) . 7_575 ? B12 B16 B11 107.8(3) . 7_575 ? B12 B16 B11 60.2(2) 7_575 7_575 ? B12 B16 B11 60.2(2) . . ? B12 B16 B11 107.8(3) 7_575 . ? B11 B16 B11 59.6(3) 7_575 . ? B12 B16 B17 59.8(2) . . ? B12 B16 B17 59.8(2) 7_575 . ? B11 B16 B17 108.1(3) 7_575 . ? B11 B16 B17 108.1(3) . . ? B12 B16 H16 122.0 . . ? B12 B16 H16 122.0 7_575 . ? B11 B16 H16 121.7 7_575 . ? B11 B16 H16 121.7 . . ? B17 B16 H16 121.7 . . ? B12 B17 B12 107.5(4) 7_575 . ? B12 B17 B16 59.8(2) 7_575 . ? B12 B17 B16 59.8(2) . . ? B12 B17 B13 107.9(3) 7_575 . ? B12 B17 B13 60.14(19) . . ? B16 B17 B13 108.1(3) . . ? B12 B17 B13 60.14(19) 7_575 7_575 ? B12 B17 B13 107.9(3) . 7_575 ? B16 B17 B13 108.1(3) . 7_575 ? B13 B17 B13 59.9(3) . 7_575 ? B12 B17 H17 121.9 7_575 . ? B12 B17 H17 121.9 . . ? B16 B17 H17 121.7 . . ? B13 B17 H17 121.6 . . ? B13 B17 H17 121.6 7_575 . ? C7 B18 B22 58.29(19) . . ? C7 B18 B18 104.18(15) . 7_575 ? B22 B18 B18 59.97(14) . 7_575 ? C7 B18 B23 104.5(3) . . ? B22 B18 B23 108.0(3) . . ? B18 B18 B23 60.06(15) 7_575 . ? C7 B18 B19 58.76(19) . . ? B22 B18 B19 107.8(3) . . ? B18 B18 B19 107.70(16) 7_575 . ? B23 B18 B19 59.8(2) . . ? C7 B18 H18 125.1 . . ? B22 B18 H18 121.6 . . ? B18 B18 H18 122.6 7_575 . ? B23 B18 H18 122.4 . . ? B19 B18 H18 121.6 . . ? C7 B19 B23 104.6(3) . . ? C7 B19 B24 104.7(3) . . ? B23 B19 B24 60.6(3) . . ? C7 B19 B20 58.78(19) . . ? B23 B19 B20 108.4(3) . . ? B24 B19 B20 59.9(3) . . ? C7 B19 B18 58.65(19) . . ? B23 B19 B18 60.0(3) . . ? B24 B19 B18 108.7(3) . . ? B20 B19 B18 108.4(2) . . ? C7 B19 H19 125.0 . . ? B23 B19 H19 122.2 . . ? B24 B19 H19 122.0 . . ? B20 B19 H19 121.3 . . ? B18 B19 H19 121.2 . . ? C7 B20 B20 104.37(15) . 7_575 ? C7 B20 B21 58.21(19) . . ? B20 B20 B21 60.08(14) 7_575 . ? C7 B20 B24 104.8(3) . . ? B20 B20 B24 60.19(15) 7_575 . ? B21 B20 B24 108.2(3) . . ? C7 B20 B19 58.81(19) . . ? B20 B20 B19 107.94(16) 7_575 . ? B21 B20 B19 107.8(3) . . ? B24 B20 B19 60.0(2) . . ? C7 B20 H20 125.0 . . ? B20 B20 H20 122.4 7_575 . ? B21 B20 H20 121.6 . . ? B24 B20 H20 122.1 . . ? B19 B20 H20 121.5 . . ? C7 B21 C7 101.0(3) . 7_575 ? C7 B21 B20 59.36(19) . . ? C7 B21 B20 105.1(3) 7_575 . ? C7 B21 B20 105.1(3) . 7_575 ? C7 B21 B20 59.36(19) 7_575 7_575 ? B20 B21 B20 59.8(3) . 7_575 ? C7 B21 B22 58.31(18) . . ? C7 B21 B22 58.31(18) 7_575 . ? B20 B21 B22 108.3(3) . . ? B20 B21 B22 108.3(3) 7_575 . ? C7 B21 H21 125.4 . . ? C7 B21 H21 125.4 7_575 . ? B20 B21 H21 121.7 . . ? B20 B21 H21 121.7 7_575 . ? B22 B21 H21 121.4 . . ? C7 B22 C7 100.6(3) 7_575 . ? C7 B22 B18 104.9(3) 7_575 . ? C7 B22 B18 59.11(19) . . ? C7 B22 B18 59.11(19) 7_575 7_575 ? C7 B22 B18 104.9(3) . 7_575 ? B18 B22 B18 60.1(3) . 7_575 ? C7 B22 B21 58.06(18) 7_575 . ? C7 B22 B21 58.06(18) . . ? B18 B22 B21 107.8(3) . . ? B18 B22 B21 107.8(3) 7_575 . ? C7 B22 H22 125.7 7_575 . ? C7 B22 H22 125.7 . . ? B18 B22 H22 121.9 . . ? B18 B22 H22 121.9 7_575 . ? B21 B22 H22 121.8 . . ? B19 B23 B19 107.3(4) 7_575 . ? B19 B23 B18 60.2(2) 7_575 7_575 ? B19 B23 B18 107.9(3) . 7_575 ? B19 B23 B18 107.9(3) 7_575 . ? B19 B23 B18 60.2(2) . . ? B18 B23 B18 59.9(3) 7_575 . ? B19 B23 B24 59.7(2) 7_575 . ? B19 B23 B24 59.7(2) . . ? B18 B23 B24 108.1(3) 7_575 . ? B18 B23 B24 108.1(3) . . ? B19 B23 H23 122.0 7_575 . ? B19 B23 H23 122.0 . . ? B18 B23 H23 121.6 7_575 . ? B18 B23 H23 121.6 . . ? B24 B23 H23 121.8 . . ? B20 B24 B20 59.6(3) 7_575 . ? B20 B24 B19 60.2(2) 7_575 7_575 ? B20 B24 B19 107.6(3) . 7_575 ? B20 B24 B19 107.6(3) 7_575 . ? B20 B24 B19 60.2(2) . . ? B19 B24 B19 107.3(4) 7_575 . ? B20 B24 B23 107.9(3) 7_575 . ? B20 B24 B23 107.9(3) . . ? B19 B24 B23 59.7(2) 7_575 . ? B19 B24 B23 59.7(2) . . ? B20 B24 H24 121.8 7_575 . ? B20 B24 H24 121.8 . . ? B19 B24 H24 122.0 7_575 . ? B19 B24 H24 122.0 . . ? B23 B24 H24 121.9 . . ? C2 C1 B1 116.5(2) . . ? C2 C1 B2 118.0(2) . . ? B1 C1 B2 63.42(19) . . ? C2 C1 B3 118.9(3) . . ? B1 C1 B3 115.0(2) . . ? B2 C1 B3 62.3(2) . . ? C2 C1 B5 116.9(2) . . ? B1 C1 B5 62.6(2) . . ? B2 C1 B5 114.9(2) . . ? B3 C1 B5 114.7(2) . . ? C2 C1 B4 119.1(2) . . ? B1 C1 B4 113.8(2) . . ? B2 C1 B4 113.9(2) . . ? B3 C1 B4 62.8(2) . . ? B5 C1 B4 62.1(2) . . ? O2 C2 O1 127.3(3) . . ? O2 C2 C1 116.3(3) . . ? O1 C2 C1 116.4(3) . . ? C4 C3 B2 118.1(2) . . ? C4 C3 B1 117.1(2) . . ? B2 C3 B1 63.61(19) . . ? C4 C3 B10 118.5(2) . . ? B2 C3 B10 114.0(2) . . ? B1 C3 B10 113.8(2) . . ? C4 C3 B9 116.9(2) . . ? B2 C3 B9 114.9(2) . . ? B1 C3 B9 62.1(2) . . ? B10 C3 B9 62.5(2) . . ? C4 C3 B6 118.8(2) . . ? B2 C3 B6 62.2(2) . . ? B1 C3 B6 114.8(2) . . ? B10 C3 B6 62.6(2) . . ? B9 C3 B6 114.7(3) . . ? O4 C4 O3 127.4(3) . . ? O4 C4 C3 116.9(3) . . ? O3 C4 C3 115.6(3) . . ? C6 C5 B15 116.0(3) . . ? C6 C5 B14 115.6(2) . . ? B15 C5 B14 63.3(2) . . ? C6 C5 B13 117.7(2) . . ? B15 C5 B13 115.2(2) . . ? B14 C5 B13 62.6(2) . . ? C6 C5 B11 118.6(2) . . ? B15 C5 B11 62.6(2) . . ? B14 C5 B11 115.2(2) . . ? B13 C5 B11 115.0(2) . . ? C6 C5 B12 120.4(2) . . ? B15 C5 B12 114.3(3) . . ? B14 C5 B12 114.3(3) . . ? B13 C5 B12 62.7(2) . . ? B11 C5 B12 62.6(2) . . ? O6 C6 O5 127.3(3) . . ? O6 C6 C5 117.3(3) . . ? O5 C6 C5 115.4(3) . . ? C8 C7 B21 115.6(2) . . ? C8 C7 B22 115.6(3) . . ? B21 C7 B22 63.6(2) . . ? C8 C7 B18 118.4(2) . . ? B21 C7 B18 115.2(2) . . ? B22 C7 B18 62.6(2) . . ? C8 C7 B20 118.3(2) . . ? B21 C7 B20 62.4(2) . . ? B22 C7 B20 115.2(2) . . ? B18 C7 B20 114.6(2) . . ? C8 C7 B19 120.5(2) . . ? B21 C7 B19 114.2(3) . . ? B22 C7 B19 114.5(3) . . ? B18 C7 B19 62.6(2) . . ? B20 C7 B19 62.4(2) . . ? O8 C8 O7 127.6(3) . . ? O8 C8 C7 116.8(3) . . ? O7 C8 C7 115.6(3) . . ? O9 C9 H9A 109.5 . . ? O9 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O9 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O10 C10 H10A 109.5 . . ? O10 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O10 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O11 C11 H11A 109.5 . . ? O11 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O11 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O12 C12 H12A 109.5 . . ? O12 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O12 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O13 C13 H13A 109.5 . . ? O13 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O13 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O14 C14 H14A 109.5 . . ? O14 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O14 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 O11 H11D 109.5 . . ? C12 O12 H12D 102.7 . . ? C13 O13 H13D 125.2 . . ? C14 O14 H14D 105.7 . . ? C15 O15 H15A 120.4 . . ? O15 C15 H15B 109.5 . . ? O15 C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O15 C15 H15D 109.5 . . ? H15B C15 H15D 109.5 . . ? H15C C15 H15D 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O11 H11D O9 0.84 2.18 2.882(5) 140.9 5_666 O10 H10D O12 0.85 1.89 2.738(5) 179.2 4_565 O13 H13D O12 0.85 1.81 2.658(9) 179.9 . O12 H12D O15 0.89 2.13 2.816(11) 134.0 . O14 H14D O10 0.85 1.80 2.652(4) 178.9 4_564 O9 H9' O13 0.82 1.90 2.698(7) 163.4 5_666 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.864 _refine_diff_density_min -0.792 _refine_diff_density_rms 0.111 # Attachment '- 3_rev_Compound-7.cif' data_mo_10325a _database_code_depnum_ccdc_archive 'CCDC 873640' #TrackingRef '- 3_rev_Compound-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H62 B20 Cu3 O20' _chemical_formula_weight 1029.52 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' O O 0.0106 0.0060 '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' Cu Cu 0.3201 1.2651 '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 9.7985(11) _cell_length_b 11.4767(13) _cell_length_c 12.2068(14) _cell_angle_alpha 110.917(2) _cell_angle_beta 103.992(2) _cell_angle_gamma 102.050(2) _cell_volume 1176.4(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3343 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 28.30 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 529 _exptl_absorpt_coefficient_mu 1.410 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6610 _exptl_absorpt_correction_T_max 0.8955 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.13 _diffrn_reflns_number 9163 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.33 _reflns_number_total 5760 _reflns_number_gt 4503 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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. In the refinement, 4 DFIX instructions were used to restrain the hydroxy groups of four methanol molecules ; _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^)+(0.1153P)^2^+0.8651P] 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 5760 _refine_ls_number_parameters 310 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1796 _refine_ls_wR_factor_gt 0.1272 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 Cu1 Cu 0.45193(5) 1.18565(4) 0.36389(4) 0.01891(15) Uani 1 1 d . . . Cu2 Cu 0.5000 1.0000 0.5000 0.01967(17) Uani 1 2 d S . . O1 O 0.4341(3) 0.8830(3) 0.3154(2) 0.0250(6) Uani 1 1 d . . . O2 O 0.4108(3) 1.0189(3) 0.2232(2) 0.0250(6) Uani 1 1 d . . . O3 O 0.4500(3) 0.7244(3) -0.2805(2) 0.0212(5) Uani 1 1 d . . . O4 O 0.2662(3) 0.8118(3) -0.2837(3) 0.0305(6) Uani 1 1 d . . . O5 O 0.3792(3) 1.1021(3) 0.4582(2) 0.0195(5) Uani 1 1 d . . . O6 O 0.4836(3) 1.3532(3) 0.5054(2) 0.0232(5) Uani 1 1 d D . . H6' H 0.567(3) 1.407(4) 0.527(5) 0.031(13) Uiso 1 1 d D . . O7 O 0.2237(3) 1.2073(3) 0.2568(3) 0.0274(6) Uani 1 1 d D . . H7' H 0.152(5) 1.164(5) 0.262(6) 0.058(19) Uiso 1 1 d D . . O8 O 0.2902(4) 0.8595(4) 0.5162(3) 0.0359(7) Uani 1 1 d . . . H8' H 0.286(8) 0.862(8) 0.575(7) 0.08(2) Uiso 1 1 d . . . B3 B 0.2766(5) 0.8234(4) -0.0305(4) 0.0204(8) Uani 1 1 d . . . H3 H 0.2688 0.9208 -0.0263 0.024 Uiso 1 1 calc R . . B4 B 0.1591(4) 0.7298(5) 0.0175(4) 0.0240(8) Uani 1 1 d . . . H4 H 0.0750 0.7651 0.0560 0.029 Uiso 1 1 calc R . . B5 B 0.2579(5) 0.6385(4) 0.0756(4) 0.0244(8) Uani 1 1 d . . . H5 H 0.2372 0.6128 0.1518 0.029 Uiso 1 1 calc R . . B6 B 0.4400(5) 0.6808(4) 0.0697(4) 0.0220(8) Uani 1 1 d . . . H6 H 0.5386 0.6841 0.1414 0.026 Uiso 1 1 calc R . . B7 B 0.4516(4) 0.7955(4) 0.0025(4) 0.0192(7) Uani 1 1 d . . . H7 H 0.5587 0.8742 0.0289 0.023 Uiso 1 1 calc R . . B8 B 0.1392(5) 0.6761(5) -0.1425(4) 0.0264(9) Uani 1 1 d . . . H8 H 0.0408 0.6747 -0.2131 0.032 Uiso 1 1 calc R . . B9 B 0.1269(5) 0.5610(5) -0.0776(4) 0.0316(10) Uani 1 1 d . . . H9 H 0.0188 0.4832 -0.1047 0.038 Uiso 1 1 calc R . . B10 B 0.3007(5) 0.5312(4) -0.0446(4) 0.0270(9) Uani 1 1 d . . . H10 H 0.3077 0.4334 -0.0496 0.032 Uiso 1 1 calc R . . B11 B 0.4211(5) 0.6274(4) -0.0909(4) 0.0231(8) Uani 1 1 d . . . H11 H 0.5073 0.5943 -0.1275 0.028 Uiso 1 1 calc R . . B12 B 0.2283(5) 0.5528(4) -0.1812(4) 0.0251(9) Uani 1 1 d . . . H12 H 0.1884 0.4705 -0.2773 0.030 Uiso 1 1 calc R . . C1 C 0.3466(4) 0.7945(3) 0.0954(3) 0.0172(6) Uani 1 1 d . . . C2 C 0.3193(4) 0.7147(4) -0.1423(3) 0.0191(7) Uani 1 1 d . . . C3 C 0.4029(4) 0.9097(4) 0.2245(3) 0.0193(7) Uani 1 1 d . . . C4 C 0.3469(4) 0.7553(4) -0.2445(3) 0.0216(7) Uani 1 1 d . . . C5 C 0.3364(4) 1.1915(4) 0.5476(3) 0.0256(8) Uani 1 1 d . . . H5A H 0.3253 1.1601 0.6117 0.031 Uiso 1 1 calc R . . H5B H 0.2400 1.1980 0.5061 0.031 Uiso 1 1 calc R . . C6 C 0.4579(5) 1.3272(4) 0.6091(3) 0.0265(8) Uani 1 1 d . . . H6A H 0.4243 1.3959 0.6605 0.032 Uiso 1 1 calc R . . H6B H 0.5502 1.3255 0.6631 0.032 Uiso 1 1 calc R . . C7 C 0.1925(5) 1.1766(5) 0.1269(4) 0.0393(11) Uani 1 1 d . . . H7A H 0.2763 1.1565 0.1028 0.059 Uiso 1 1 calc R . . H7B H 0.1778 1.2523 0.1122 0.059 Uiso 1 1 calc R . . H7C H 0.1022 1.0999 0.0768 0.059 Uiso 1 1 calc R . . C8 C 0.1578(6) 0.7789(7) 0.4111(5) 0.0552(15) Uani 1 1 d . . . H8A H 0.1491 0.8156 0.3495 0.083 Uiso 1 1 calc R . . H8B H 0.0714 0.7764 0.4383 0.083 Uiso 1 1 calc R . . H8C H 0.1619 0.6892 0.3732 0.083 Uiso 1 1 calc R . . C9 C 0.0853(9) 0.0375(8) 0.7385(10) 0.088(3) Uani 1 1 d . . . H9A H 0.1142 0.1028 0.8251 0.133 Uiso 1 1 calc R . . H9B H 0.0062 0.0529 0.6845 0.133 Uiso 1 1 calc R . . H9C H 0.1717 0.0456 0.7113 0.133 Uiso 1 1 calc R . . O9 O 0.0342(4) -0.0884(5) 0.7310(5) 0.0692(14) Uani 1 1 d D . . H9' H 0.117(4) -0.092(6) 0.765(5) 0.049(16) Uiso 1 1 d D . . C10 C 0.1699(6) 0.4644(6) 0.4648(5) 0.0459(12) Uani 1 1 d . . . H10A H 0.2308 0.4598 0.5387 0.069 Uiso 1 1 calc R . . H10B H 0.0803 0.3865 0.4200 0.069 Uiso 1 1 calc R . . H10C H 0.1413 0.5442 0.4908 0.069 Uiso 1 1 calc R . . O10 O 0.2520(3) 0.4684(3) 0.3859(3) 0.0366(7) Uani 1 1 d D . . H10' H 0.245(7) 0.384(3) 0.325(5) 0.060(18) Uiso 1 1 d 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 Cu1 0.0261(2) 0.0225(2) 0.0126(2) 0.00856(18) 0.01086(17) 0.00986(18) Cu2 0.0316(3) 0.0225(3) 0.0077(3) 0.0075(2) 0.0079(2) 0.0113(3) O1 0.0427(15) 0.0245(13) 0.0096(11) 0.0081(10) 0.0077(11) 0.0146(12) O2 0.0417(15) 0.0209(13) 0.0141(12) 0.0079(10) 0.0122(11) 0.0103(11) O3 0.0263(13) 0.0244(13) 0.0177(12) 0.0097(10) 0.0131(10) 0.0099(10) O4 0.0329(15) 0.0535(19) 0.0241(14) 0.0281(14) 0.0159(12) 0.0232(14) O5 0.0261(12) 0.0242(13) 0.0117(11) 0.0088(10) 0.0090(10) 0.0099(10) O6 0.0296(14) 0.0245(13) 0.0145(12) 0.0072(10) 0.0081(11) 0.0086(11) O7 0.0230(13) 0.0360(16) 0.0209(14) 0.0100(12) 0.0073(11) 0.0091(12) O8 0.0344(16) 0.052(2) 0.0223(15) 0.0218(15) 0.0086(13) 0.0060(14) B3 0.0248(18) 0.028(2) 0.0119(17) 0.0096(15) 0.0085(14) 0.0120(16) B4 0.0200(18) 0.035(2) 0.0168(19) 0.0111(17) 0.0084(15) 0.0060(17) B5 0.032(2) 0.023(2) 0.019(2) 0.0101(16) 0.0123(17) 0.0042(17) B6 0.029(2) 0.027(2) 0.0155(18) 0.0106(16) 0.0105(16) 0.0120(17) B7 0.0209(18) 0.026(2) 0.0123(17) 0.0085(15) 0.0080(14) 0.0082(15) B8 0.0207(19) 0.041(3) 0.0147(18) 0.0117(18) 0.0059(15) 0.0053(17) B9 0.030(2) 0.039(3) 0.017(2) 0.0093(19) 0.0085(17) -0.0015(19) B10 0.043(2) 0.021(2) 0.0165(19) 0.0078(16) 0.0111(18) 0.0078(18) B11 0.031(2) 0.026(2) 0.0161(19) 0.0096(16) 0.0107(16) 0.0128(17) B12 0.033(2) 0.023(2) 0.0139(18) 0.0058(16) 0.0092(16) 0.0021(17) C1 0.0210(15) 0.0233(17) 0.0091(14) 0.0076(13) 0.0070(12) 0.0074(13) C2 0.0205(16) 0.0269(18) 0.0120(15) 0.0093(13) 0.0079(13) 0.0076(14) C3 0.0228(16) 0.0258(18) 0.0095(15) 0.0075(13) 0.0062(13) 0.0079(14) C4 0.0275(17) 0.0276(18) 0.0129(16) 0.0103(14) 0.0107(14) 0.0080(15) C5 0.0290(18) 0.039(2) 0.0173(17) 0.0130(16) 0.0143(15) 0.0181(17) C6 0.039(2) 0.033(2) 0.0119(16) 0.0088(15) 0.0109(15) 0.0182(17) C7 0.032(2) 0.062(3) 0.023(2) 0.016(2) 0.0069(17) 0.021(2) C8 0.039(3) 0.077(4) 0.044(3) 0.033(3) 0.006(2) 0.004(3) C9 0.083(5) 0.069(5) 0.156(9) 0.070(6) 0.068(6) 0.038(4) O9 0.040(2) 0.073(3) 0.143(5) 0.076(3) 0.053(3) 0.036(2) C10 0.048(3) 0.047(3) 0.031(2) 0.009(2) 0.012(2) 0.009(2) O10 0.0364(16) 0.0335(17) 0.0349(17) 0.0109(14) 0.0111(14) 0.0100(13) _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 O5 1.911(2) . ? Cu1 O2 1.942(3) . ? Cu1 O3 1.958(2) 2_675 ? Cu1 O6 1.974(3) . ? Cu1 O7 2.413(3) . ? Cu2 O5 1.936(2) . ? Cu2 O5 1.936(2) 2_676 ? Cu2 O1 2.018(2) 2_676 ? Cu2 O1 2.018(2) . ? Cu2 O8 2.430(3) . ? Cu2 O8 2.430(3) 2_676 ? O1 C3 1.239(4) . ? O2 C3 1.245(4) . ? O3 C4 1.262(4) . ? O3 Cu1 1.958(2) 2_675 ? O4 C4 1.237(5) . ? O5 C5 1.421(4) . ? O6 C6 1.465(4) . ? O6 H6' 0.829(19) . ? O7 C7 1.433(5) . ? O7 H7' 0.80(2) . ? O8 C8 1.425(6) . ? O8 H8' 0.72(7) . ? B3 C2 1.695(5) . ? B3 C1 1.701(5) . ? B3 B8 1.747(6) . ? B3 B4 1.756(6) . ? B3 B7 1.787(6) . ? B3 H3 1.1200 . ? B4 C1 1.707(5) . ? B4 B8 1.772(6) . ? B4 B5 1.777(6) . ? B4 B9 1.778(7) . ? B4 H4 1.1200 . ? B5 C1 1.720(5) . ? B5 B10 1.752(6) . ? B5 B9 1.763(6) . ? B5 B6 1.776(6) . ? B5 H5 1.1200 . ? B6 C1 1.727(5) . ? B6 B10 1.774(6) . ? B6 B7 1.780(6) . ? B6 B11 1.780(6) . ? B6 H6 1.1200 . ? B7 C2 1.699(5) . ? B7 C1 1.706(5) . ? B7 B11 1.770(6) . ? B7 H7 1.1200 . ? B8 C2 1.726(5) . ? B8 B9 1.765(7) . ? B8 B12 1.796(7) . ? B8 H8 1.1200 . ? B9 B12 1.777(6) . ? B9 B10 1.786(7) . ? B9 H9 1.1200 . ? B10 B12 1.772(6) . ? B10 B11 1.775(6) . ? B10 H10 1.1200 . ? B11 C2 1.719(5) . ? B11 B12 1.778(6) . ? B11 H11 1.1200 . ? B12 C2 1.716(6) . ? B12 H12 1.1200 . ? C1 C3 1.525(5) . ? C2 C4 1.540(5) . ? C5 C6 1.538(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 O9 1.388(8) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? O9 H9' 0.83(2) . ? C10 O10 1.403(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? O10 H10' 0.96(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 O5 Cu1 O2 93.18(11) . . ? O5 Cu1 O3 173.24(11) . 2_675 ? O2 Cu1 O3 88.60(11) . 2_675 ? O5 Cu1 O6 85.67(11) . . ? O2 Cu1 O6 177.31(11) . . ? O3 Cu1 O6 92.82(11) 2_675 . ? O5 Cu1 O7 98.89(10) . . ? O2 Cu1 O7 90.00(11) . . ? O3 Cu1 O7 87.63(10) 2_675 . ? O6 Cu1 O7 87.78(10) . . ? O5 Cu2 O5 179.999(1) . 2_676 ? O5 Cu2 O1 92.05(10) . 2_676 ? O5 Cu2 O1 87.95(10) 2_676 2_676 ? O5 Cu2 O1 87.95(10) . . ? O5 Cu2 O1 92.05(10) 2_676 . ? O1 Cu2 O1 179.999(1) 2_676 . ? O5 Cu2 O8 90.33(11) . . ? O5 Cu2 O8 89.67(11) 2_676 . ? O1 Cu2 O8 89.55(11) 2_676 . ? O1 Cu2 O8 90.45(11) . . ? O5 Cu2 O8 89.67(11) . 2_676 ? O5 Cu2 O8 90.33(11) 2_676 2_676 ? O1 Cu2 O8 90.45(11) 2_676 2_676 ? O1 Cu2 O8 89.55(11) . 2_676 ? O8 Cu2 O8 180.0 . 2_676 ? C3 O1 Cu2 130.3(2) . . ? C3 O2 Cu1 127.7(2) . . ? C4 O3 Cu1 121.5(2) . 2_675 ? C5 O5 Cu1 109.3(2) . . ? C5 O5 Cu2 122.8(2) . . ? Cu1 O5 Cu2 111.32(12) . . ? C6 O6 Cu1 109.8(2) . . ? C6 O6 H6' 112(4) . . ? Cu1 O6 H6' 112(4) . . ? C7 O7 Cu1 116.5(2) . . ? C7 O7 H7' 107(5) . . ? Cu1 O7 H7' 113(5) . . ? C8 O8 Cu2 121.7(3) . . ? C8 O8 H8' 115(6) . . ? Cu2 O8 H8' 123(6) . . ? C2 B3 C1 101.9(3) . . ? C2 B3 B8 60.2(2) . . ? C1 B3 B8 106.1(3) . . ? C2 B3 B4 106.6(3) . . ? C1 B3 B4 59.1(2) . . ? B8 B3 B4 60.8(2) . . ? C2 B3 B7 58.3(2) . . ? C1 B3 B7 58.5(2) . . ? B8 B3 B7 109.0(3) . . ? B4 B3 B7 108.5(3) . . ? C2 B3 H3 124.6 . . ? C1 B3 H3 125.2 . . ? B8 B3 H3 120.8 . . ? B4 B3 H3 121.3 . . ? B7 B3 H3 121.4 . . ? C1 B4 B3 58.8(2) . . ? C1 B4 B8 104.7(3) . . ? B3 B4 B8 59.3(2) . . ? C1 B4 B5 59.1(2) . . ? B3 B4 B5 107.6(3) . . ? B8 B4 B5 107.2(3) . . ? C1 B4 B9 104.8(3) . . ? B3 B4 B9 106.9(3) . . ? B8 B4 B9 59.6(3) . . ? B5 B4 B9 59.5(3) . . ? C1 B4 H4 124.2 . . ? B3 B4 H4 122.0 . . ? B8 B4 H4 122.8 . . ? B5 B4 H4 121.8 . . ? B9 B4 H4 122.8 . . ? C1 B5 B10 105.4(3) . . ? C1 B5 B9 104.9(3) . . ? B10 B5 B9 61.1(3) . . ? C1 B5 B6 59.2(2) . . ? B10 B5 B6 60.4(3) . . ? B9 B5 B6 109.4(3) . . ? C1 B5 B4 58.4(2) . . ? B10 B5 B4 109.3(3) . . ? B9 B5 B4 60.3(3) . . ? B6 B5 B4 108.9(3) . . ? C1 B5 H5 124.9 . . ? B10 B5 H5 121.5 . . ? B9 B5 H5 121.7 . . ? B6 B5 H5 120.7 . . ? B4 B5 H5 121.1 . . ? C1 B6 B10 104.1(3) . . ? C1 B6 B5 58.8(2) . . ? B10 B6 B5 59.2(2) . . ? C1 B6 B7 58.2(2) . . ? B10 B6 B7 107.2(3) . . ? B5 B6 B7 107.1(3) . . ? C1 B6 B11 104.1(3) . . ? B10 B6 B11 59.9(2) . . ? B5 B6 B11 107.1(3) . . ? B7 B6 B11 59.6(2) . . ? C1 B6 H6 125.0 . . ? B10 B6 H6 122.8 . . ? B5 B6 H6 122.1 . . ? B7 B6 H6 122.0 . . ? B11 B6 H6 122.7 . . ? C2 B7 C1 101.5(3) . . ? C2 B7 B11 59.4(2) . . ? C1 B7 B11 105.4(3) . . ? C2 B7 B6 105.5(3) . . ? C1 B7 B6 59.4(2) . . ? B11 B7 B6 60.2(2) . . ? C2 B7 B3 58.1(2) . . ? C1 B7 B3 58.2(2) . . ? B11 B7 B3 107.8(3) . . ? B6 B7 B3 107.9(3) . . ? C2 B7 H7 125.1 . . ? C1 B7 H7 125.1 . . ? B11 B7 H7 121.7 . . ? B6 B7 H7 121.6 . . ? B3 B7 H7 121.9 . . ? C2 B8 B3 58.4(2) . . ? C2 B8 B9 104.4(3) . . ? B3 B8 B9 107.9(3) . . ? C2 B8 B4 104.5(3) . . ? B3 B8 B4 59.9(2) . . ? B9 B8 B4 60.4(3) . . ? C2 B8 B12 58.3(2) . . ? B3 B8 B12 107.3(3) . . ? B9 B8 B12 59.9(3) . . ? B4 B8 B12 107.9(3) . . ? C2 B8 H8 125.1 . . ? B3 B8 H8 121.8 . . ? B9 B8 H8 122.2 . . ? B4 B8 H8 122.2 . . ? B12 B8 H8 121.9 . . ? B5 B9 B8 108.1(3) . . ? B5 B9 B12 107.2(3) . . ? B8 B9 B12 60.9(3) . . ? B5 B9 B4 60.3(2) . . ? B8 B9 B4 60.0(3) . . ? B12 B9 B4 108.5(3) . . ? B5 B9 B10 59.2(3) . . ? B8 B9 B10 108.5(3) . . ? B12 B9 B10 59.7(3) . . ? B4 B9 B10 107.8(3) . . ? B5 B9 H9 122.2 . . ? B8 B9 H9 121.1 . . ? B12 B9 H9 121.6 . . ? B4 B9 H9 121.5 . . ? B10 B9 H9 122.1 . . ? B5 B10 B12 107.9(3) . . ? B5 B10 B6 60.5(2) . . ? B12 B10 B6 108.5(3) . . ? B5 B10 B11 108.3(3) . . ? B12 B10 B11 60.2(2) . . ? B6 B10 B11 60.2(2) . . ? B5 B10 B9 59.8(3) . . ? B12 B10 B9 59.9(3) . . ? B6 B10 B9 108.4(3) . . ? B11 B10 B9 108.1(3) . . ? B5 B10 H10 121.7 . . ? B12 B10 H10 121.7 . . ? B6 B10 H10 121.2 . . ? B11 B10 H10 121.5 . . ? B9 B10 H10 121.7 . . ? C2 B11 B7 58.2(2) . . ? C2 B11 B10 104.4(3) . . ? B7 B11 B10 107.6(3) . . ? C2 B11 B12 58.7(2) . . ? B7 B11 B12 107.6(3) . . ? B10 B11 B12 59.8(2) . . ? C2 B11 B6 104.7(3) . . ? B7 B11 B6 60.2(2) . . ? B10 B11 B6 59.9(2) . . ? B12 B11 B6 108.0(3) . . ? C2 B11 H11 124.9 . . ? B7 B11 H11 121.8 . . ? B10 B11 H11 122.6 . . ? B12 B11 H11 121.6 . . ? B6 B11 H11 122.2 . . ? C2 B12 B10 104.7(3) . . ? C2 B12 B9 104.4(3) . . ? B10 B12 B9 60.4(3) . . ? C2 B12 B11 58.9(2) . . ? B10 B12 B11 60.0(2) . . ? B9 B12 B11 108.4(3) . . ? C2 B12 B8 58.8(2) . . ? B10 B12 B8 107.7(3) . . ? B9 B12 B8 59.2(3) . . ? B11 B12 B8 108.3(3) . . ? C2 B12 H12 124.8 . . ? B10 B12 H12 122.3 . . ? B9 B12 H12 122.5 . . ? B11 B12 H12 121.1 . . ? B8 B12 H12 121.7 . . ? C3 C1 B3 117.7(3) . . ? C3 C1 B7 117.5(3) . . ? B3 C1 B7 63.3(2) . . ? C3 C1 B4 117.6(3) . . ? B3 C1 B4 62.1(2) . . ? B7 C1 B4 114.8(3) . . ? C3 C1 B5 119.6(3) . . ? B3 C1 B5 112.9(3) . . ? B7 C1 B5 113.2(3) . . ? B4 C1 B5 62.5(2) . . ? C3 C1 B6 118.1(3) . . ? B3 C1 B6 114.5(3) . . ? B7 C1 B6 62.5(2) . . ? B4 C1 B6 114.6(3) . . ? B5 C1 B6 62.0(2) . . ? C4 C2 B3 116.1(3) . . ? C4 C2 B7 117.4(3) . . ? B3 C2 B7 63.6(2) . . ? C4 C2 B12 119.7(3) . . ? B3 C2 B12 113.5(3) . . ? B7 C2 B12 113.9(3) . . ? C4 C2 B11 119.7(3) . . ? B3 C2 B11 114.7(3) . . ? B7 C2 B11 62.4(2) . . ? B12 C2 B11 62.3(2) . . ? C4 C2 B8 117.2(3) . . ? B3 C2 B8 61.4(2) . . ? B7 C2 B8 114.3(3) . . ? B12 C2 B8 62.9(3) . . ? B11 C2 B8 114.4(3) . . ? O1 C3 O2 129.0(3) . . ? O1 C3 C1 116.7(3) . . ? O2 C3 C1 114.4(3) . . ? O4 C4 O3 127.0(3) . . ? O4 C4 C2 117.8(3) . . ? O3 C4 C2 115.2(3) . . ? O5 C5 C6 108.1(3) . . ? O5 C5 H5A 110.1 . . ? C6 C5 H5A 110.1 . . ? O5 C5 H5B 110.1 . . ? C6 C5 H5B 110.1 . . ? H5A C5 H5B 108.4 . . ? O6 C6 C5 105.5(3) . . ? O6 C6 H6A 110.7 . . ? C5 C6 H6A 110.7 . . ? O6 C6 H6B 110.7 . . ? C5 C6 H6B 110.7 . . ? H6A C6 H6B 108.8 . . ? O7 C7 H7A 109.5 . . ? O7 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O7 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O8 C8 H8A 109.5 . . ? O8 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O8 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O9 C9 H9A 109.5 . . ? O9 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O9 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C9 O9 H9' 97(4) . . ? O10 C10 H10A 109.5 . . ? O10 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O10 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C10 O10 H10' 116(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O10 H10' O7 0.96(2) 1.84(3) 2.758(4) 158(6) 1_545 O9 H9' O4 0.83(2) 2.09(4) 2.766(4) 138(5) 1_546 O8 H8' O4 0.72(7) 2.04(7) 2.738(4) 163(8) 1_556 O7 H7' O9 0.80(2) 1.88(2) 2.675(5) 169(7) 2_566 O6 H6' O10 0.829(19) 1.81(2) 2.617(4) 165(5) 2_676 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.772 _refine_diff_density_min -0.835 _refine_diff_density_rms 0.203 # Attachment '- 3_rev_Compound-8.cif' data_mo_00901c _database_code_depnum_ccdc_archive 'CCDC 873641' #TrackingRef '- 3_rev_Compound-8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H60 B20 Cu2 N4 O18' _chemical_formula_weight 988.00 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' 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' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 18.883(13) _cell_length_b 11.088(7) _cell_length_c 11.086(8) _cell_angle_alpha 90.00 _cell_angle_beta 104.588(11) _cell_angle_gamma 90.00 _cell_volume 2246(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2653 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 27.09 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1020 _exptl_absorpt_coefficient_mu 1.017 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9509 _exptl_absorpt_correction_T_max 0.9604 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEX-II CCD' _diffrn_measurement_method ' \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6330 _diffrn_reflns_av_R_equivalents 0.0819 _diffrn_reflns_av_sigmaI/netI 0.0940 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2063 _reflns_number_gt 1665 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.338 -0.022 0.022 1312 394 ' ' _platon_squeeze_details ; ; _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^)+(0.1283P)^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 2063 _refine_ls_number_parameters 159 _refine_ls_number_restraints 116 _refine_ls_R_factor_all 0.0819 _refine_ls_R_factor_gt 0.0700 _refine_ls_wR_factor_ref 0.1891 _refine_ls_wR_factor_gt 0.1830 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.003 _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 Cu1 Cu 0.57375(4) 0.5000 0.53169(7) 0.0075(3) Uani 1 2 d SU . 1 O1 O 0.5612(2) 0.6754(3) 0.5259(4) 0.0354(11) Uani 1 1 d U A 1 O2 O 0.5605(3) 0.5000 0.7001(5) 0.0294(13) Uani 1 2 d SU . 1 O3 O 0.4380(3) 0.5000 0.6483(5) 0.0305(13) Uani 1 2 d SU . 1 B1 B 0.4888(11) 0.9329(12) 0.6303(14) 0.030(3) Uani 0.50 1 d PU . 1 H1 H 0.4825 0.8874 0.7172 0.036 Uiso 0.50 1 calc PR . 1 B2 B 0.4188(7) 0.9292(11) 0.4851(17) 0.020(3) Uani 0.50 1 d PU . 1 H2 H 0.3659 0.8803 0.4769 0.025 Uiso 0.50 1 calc PR . 1 B3 B 0.4623(10) 0.9298(11) 0.3611(14) 0.027(3) Uani 0.50 1 d PU . 1 H3 H 0.4388 0.8826 0.2705 0.032 Uiso 0.50 1 calc PR . 1 B4 B 0.5629(9) 0.9361(12) 0.4361(18) 0.027(3) Uani 0.50 1 d PU . 1 H4 H 0.6049 0.8919 0.3953 0.032 Uiso 0.50 1 calc PR . 1 B5 B 0.5746(8) 0.9387(12) 0.5935(17) 0.026(3) Uani 0.50 1 d PU . 1 H5 H 0.6239 0.8947 0.6554 0.031 Uiso 0.50 1 calc PR . 1 B6 B 0.5529(11) 0.3994(15) 0.9541(16) 0.032(4) Uani 0.50 1 d PU . 1 H6 H 0.5994 0.3354 0.9588 0.039 Uiso 0.50 1 calc PR . 1 B7 B 0.4590(10) 0.3808(15) 0.9159(14) 0.027(4) Uani 0.50 1 d PU . 1 H7 H 0.4330 0.3014 0.8594 0.032 Uiso 0.50 1 calc PR . 1 B8 B 0.4203(6) 0.5262(11) 0.9005(10) 0.020(4) Uani 0.50 1 d PU . 1 H8 H 0.3667 0.5436 0.8317 0.024 Uiso 0.50 1 calc PR . 1 B9 B 0.4952(12) 0.6321(15) 0.9311(16) 0.031(4) Uani 0.50 1 d PU . 1 H9 H 0.4922 0.7214 0.8827 0.037 Uiso 0.50 1 calc PR . 1 B10 B 0.5759(9) 0.5493(18) 0.9635(14) 0.033(4) Uani 0.50 1 d PU . 1 H10 H 0.6268 0.5802 0.9381 0.040 Uiso 0.50 1 calc PR . 1 C1 C 0.5000 0.8614(6) 0.5000 0.0151(14) Uani 1 2 d SU . 1 C2 C 0.5000 0.7235(6) 0.5000 0.0164(15) Uani 1 2 d SU . 1 C3 C 0.4995(4) 0.5000 0.8608(6) 0.0163(15) Uani 1 2 d SU . 1 C4 C 0.4989(4) 0.5000 0.7239(6) 0.0162(15) Uani 1 2 d SU . 1 O4 O 0.6862(3) 0.5289(6) 0.5813(8) 0.030(2) Uani 0.50 1 d PDU . . H4A H 0.7140 0.5914 0.6050 0.036 Uiso 0.50 1 d PRD . . H4B H 0.6994 0.5000 0.5170 0.036 Uiso 1 2 d SRD . . 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 0.0130(5) 0.0032(4) 0.0066(4) 0.000 0.0033(3) 0.000 O1 0.035(2) 0.0134(18) 0.058(3) 0.0019(17) 0.012(2) 0.0069(16) O2 0.028(3) 0.050(3) 0.011(3) 0.000 0.006(2) 0.000 O3 0.024(3) 0.048(3) 0.020(3) 0.000 0.005(2) 0.000 B1 0.052(8) 0.017(6) 0.028(6) -0.002(5) 0.023(6) 0.000(6) B2 0.022(6) 0.013(5) 0.025(7) 0.003(5) 0.005(6) 0.003(4) B3 0.036(7) 0.012(6) 0.030(6) 0.000(5) 0.003(6) 0.003(5) B4 0.039(7) 0.019(5) 0.034(7) 0.005(5) 0.029(6) 0.001(5) B5 0.022(6) 0.018(5) 0.030(7) -0.001(5) -0.007(6) -0.001(5) B6 0.049(9) 0.025(7) 0.026(7) 0.006(6) 0.013(6) 0.018(6) B7 0.036(7) 0.032(7) 0.012(6) -0.003(5) 0.005(6) -0.023(7) B8 0.018(4) 0.034(10) 0.008(4) 0.006(4) 0.002(4) 0.008(5) B9 0.050(8) 0.027(6) 0.020(7) -0.001(5) 0.018(7) 0.002(7) B10 0.029(7) 0.060(9) 0.013(6) 0.004(6) 0.011(5) -0.010(6) C1 0.020(3) 0.005(3) 0.022(3) 0.000 0.008(3) 0.000 C2 0.028(4) 0.011(3) 0.013(3) 0.000 0.010(3) 0.000 C3 0.024(4) 0.015(3) 0.009(3) 0.000 0.003(3) 0.000 C4 0.025(4) 0.014(3) 0.012(3) 0.000 0.007(3) 0.000 O4 0.011(3) 0.031(7) 0.046(4) -0.005(3) 0.004(3) -0.001(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 Cu1 O2 1.946(5) . ? Cu1 O3 1.951(6) 5_666 ? Cu1 O1 1.958(4) 6_565 ? Cu1 O1 1.958(4) . ? Cu1 O4 2.080(7) . ? Cu1 O4 2.080(7) 6_565 ? Cu1 Cu1 2.696(2) 5_666 ? O1 C2 1.240(5) . ? O2 C4 1.254(9) . ? O3 C4 1.241(9) . ? O3 Cu1 1.951(6) 5_666 ? B1 C1 1.707(14) . ? B1 B3 1.771(17) 5_676 ? B1 B5 1.77(2) . ? B1 B4 1.80(2) 5_676 ? B1 B2 1.81(2) . ? B2 C1 1.678(13) . ? B2 B4 1.721(17) 5_676 ? B2 B5 1.725(18) 5_676 ? B2 B3 1.77(2) . ? B3 C1 1.703(14) . ? B3 B5 1.744(18) 5_676 ? B3 B1 1.771(17) 5_676 ? B3 B4 1.87(2) . ? B4 B5 1.70(2) . ? B4 B2 1.721(17) 5_676 ? B4 C1 1.739(13) . ? B4 B1 1.80(2) 5_676 ? B5 B2 1.725(18) 5_676 ? B5 B3 1.744(18) 5_676 ? B5 C1 1.748(13) . ? B6 B9 1.11(3) 6_565 ? B6 B10 1.71(3) . ? B6 C3 1.675(16) . ? B6 B7 1.73(2) . ? B6 B8 1.77(2) 5_667 ? B7 C3 1.715(16) . ? B7 B9 1.71(2) 5_667 ? B7 B8 1.76(2) . ? B7 B10 1.81(3) 5_667 ? B8 C3 1.688(13) . ? B8 B10 1.710(19) 5_667 ? B8 B6 1.77(2) 5_667 ? B8 B9 1.80(2) . ? B9 C3 1.671(17) . ? B9 B7 1.71(2) 5_667 ? B9 B10 1.74(2) . ? B9 B6 1.78(3) 5_667 ? B10 C3 1.688(17) . ? B10 B8 1.710(19) 5_667 ? B10 B7 1.81(3) 5_667 ? C1 C2 1.530(9) . ? C1 B2 1.678(13) 2_656 ? C1 B3 1.703(14) 2_656 ? C1 B1 1.707(14) 2_656 ? C1 B4 1.739(13) 2_656 ? C1 B5 1.748(13) 2_656 ? C2 O1 1.240(5) 2_656 ? C3 C4 1.514(10) . ? C3 B10 1.688(17) 6_565 ? C3 B9 1.671(17) 6_565 ? C3 B8 1.688(13) 6_565 ? C3 B6 1.675(16) 6_565 ? C3 B7 1.715(16) 6_565 ? O4 O4 0.642(14) 6_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 O3 166.5(2) . 5_666 ? O2 Cu1 O1 89.30(14) . 6_565 ? O3 Cu1 O1 89.12(13) 5_666 6_565 ? O2 Cu1 O1 89.30(14) . . ? O3 Cu1 O1 89.12(13) 5_666 . ? O1 Cu1 O1 166.6(2) 6_565 . ? O2 Cu1 O4 96.7(3) . . ? O3 Cu1 O4 96.7(3) 5_666 . ? O1 Cu1 O4 105.6(2) 6_565 . ? O1 Cu1 O4 87.8(2) . . ? O2 Cu1 O4 96.7(3) . 6_565 ? O3 Cu1 O4 96.7(3) 5_666 6_565 ? O1 Cu1 O4 87.8(2) 6_565 6_565 ? O1 Cu1 O4 105.6(2) . 6_565 ? O4 Cu1 O4 17.7(4) . 6_565 ? O2 Cu1 Cu1 82.85(17) . 5_666 ? O3 Cu1 Cu1 83.64(16) 5_666 5_666 ? O1 Cu1 Cu1 83.29(12) 6_565 5_666 ? O1 Cu1 Cu1 83.29(12) . 5_666 ? O4 Cu1 Cu1 171.12(19) . 5_666 ? O4 Cu1 Cu1 171.12(19) 6_565 5_666 ? C2 O1 Cu1 122.2(4) . . ? C4 O2 Cu1 123.5(5) . . ? C4 O3 Cu1 122.6(5) . 5_666 ? C1 B1 B3 105.7(9) . 5_676 ? C1 B1 B5 60.4(7) . . ? B3 B1 B5 59.1(8) 5_676 . ? C1 B1 B4 101.5(9) . 5_676 ? B3 B1 B4 63.3(8) 5_676 5_676 ? B5 B1 B4 108.1(9) . 5_676 ? C1 B1 B2 57.0(7) . . ? B3 B1 B2 108.8(9) 5_676 . ? B5 B1 B2 107.6(9) . . ? B4 B1 B2 57.0(7) 5_676 . ? C1 B2 B4 106.1(9) . 5_676 ? C1 B2 B5 104.4(9) . 5_676 ? B4 B2 B5 59.3(9) 5_676 5_676 ? C1 B2 B3 59.1(7) . . ? B4 B2 B3 108.6(9) 5_676 . ? B5 B2 B3 59.9(7) 5_676 . ? C1 B2 B1 58.5(6) . . ? B4 B2 B1 61.3(7) 5_676 . ? B5 B2 B1 107.5(9) 5_676 . ? B3 B2 B1 108.2(9) . . ? C1 B3 B5 102.6(9) . 5_676 ? C1 B3 B1 103.9(9) . 5_676 ? B5 B3 B1 60.4(8) 5_676 5_676 ? C1 B3 B2 57.8(7) . . ? B5 B3 B2 58.8(7) 5_676 . ? B1 B3 B2 107.4(9) 5_676 . ? C1 B3 B4 58.0(6) . . ? B5 B3 B4 106.0(9) 5_676 . ? B1 B3 B4 59.2(7) 5_676 . ? B2 B3 B4 105.8(9) . . ? B5 B4 B2 60.5(7) . 5_676 ? B5 B4 C1 61.0(7) . . ? B2 B4 C1 106.0(8) 5_676 . ? B5 B4 B1 108.8(9) . 5_676 ? B2 B4 B1 61.7(8) 5_676 5_676 ? C1 B4 B1 101.2(9) . 5_676 ? B5 B4 B3 108.1(9) . . ? B2 B4 B3 108.0(9) 5_676 . ? C1 B4 B3 56.1(7) . . ? B1 B4 B3 57.6(7) 5_676 . ? B4 B5 B2 60.3(8) . 5_676 ? B4 B5 B3 110.6(10) . 5_676 ? B2 B5 B3 61.4(8) 5_676 5_676 ? B4 B5 C1 60.5(7) . . ? B2 B5 C1 105.5(8) 5_676 . ? B3 B5 C1 105.1(9) 5_676 . ? B4 B5 B1 110.3(10) . . ? B2 B5 B1 109.5(10) 5_676 . ? B3 B5 B1 60.5(8) 5_676 . ? C1 B5 B1 58.1(7) . . ? B9 B6 B10 122.5(16) 6_565 . ? B9 B6 C3 70.4(12) 6_565 . ? B10 B6 C3 59.7(9) . . ? B9 B6 B7 11.5(12) 6_565 . ? B10 B6 B7 111.0(13) . . ? C3 B6 B7 60.5(9) . . ? B9 B6 B8 113.3(16) 6_565 5_667 ? B10 B6 B8 58.8(9) . 5_667 ? C3 B6 B8 104.0(9) . 5_667 ? B7 B6 B8 108.6(11) . 5_667 ? C3 B7 B9 105.0(13) . 5_667 ? C3 B7 B8 58.1(7) . . ? B9 B7 B8 105.5(12) 5_667 . ? C3 B7 B6 58.2(7) . . ? B9 B7 B6 62.2(13) 5_667 . ? B8 B7 B6 106.9(10) . . ? C3 B7 B10 102.2(11) . 5_667 ? B9 B7 B10 59.2(9) 5_667 5_667 ? B8 B7 B10 57.3(9) . 5_667 ? B6 B7 B10 108.1(11) . 5_667 ? C3 B8 B10 107.6(8) . 5_667 ? C3 B8 B7 59.6(6) . . ? B10 B8 B7 62.8(9) 5_667 . ? C3 B8 B6 104.5(9) . 5_667 ? B10 B8 B6 59.1(10) 5_667 5_667 ? B7 B8 B6 108.8(9) . 5_667 ? C3 B8 B9 57.1(7) . . ? B10 B8 B9 107.3(9) 5_667 . ? B7 B8 B9 106.9(10) . . ? B6 B8 B9 59.6(9) 5_667 . ? C3 B9 B7 108.6(15) . 5_667 ? C3 B9 B10 59.3(9) . . ? B7 B9 B10 63.3(13) 5_667 . ? C3 B9 B6 104.8(12) . 5_667 ? B7 B9 B6 59.5(9) 5_667 5_667 ? B10 B9 B6 109.2(12) . 5_667 ? C3 B9 B8 58.0(7) . . ? B7 B9 B8 108.0(12) 5_667 . ? B10 B9 B8 107.5(11) . . ? B6 B9 B8 59.2(10) 5_667 . ? C3 B10 B6 59.0(10) . . ? C3 B10 B8 106.0(10) . 5_667 ? B6 B10 B8 62.1(9) . 5_667 ? C3 B10 B9 58.4(8) . . ? B6 B10 B9 107.7(13) . . ? B8 B10 B9 106.3(11) 5_667 . ? C3 B10 B7 103.2(11) . 5_667 ? B6 B10 B7 109.0(12) . 5_667 ? B8 B10 B7 60.0(8) 5_667 5_667 ? B9 B10 B7 57.5(10) . 5_667 ? C2 C1 B2 116.6(5) . 2_656 ? C2 C1 B2 116.6(5) . . ? B2 C1 B2 126.8(9) 2_656 . ? C2 C1 B3 116.4(5) . 2_656 ? B2 C1 B3 63.1(8) 2_656 2_656 ? B2 C1 B3 93.0(8) . 2_656 ? C2 C1 B3 116.4(5) . . ? B2 C1 B3 93.0(8) 2_656 . ? B2 C1 B3 63.1(8) . . ? B3 C1 B3 127.1(9) 2_656 . ? C2 C1 B1 117.7(5) . . ? B2 C1 B1 90.8(8) 2_656 . ? B2 C1 B1 64.6(8) . . ? B3 C1 B1 30.8(7) 2_656 . ? B3 C1 B1 116.5(7) . . ? C2 C1 B1 117.7(5) . 2_656 ? B2 C1 B1 64.6(8) 2_656 2_656 ? B2 C1 B1 90.8(8) . 2_656 ? B3 C1 B1 116.5(7) 2_656 2_656 ? B3 C1 B1 30.8(7) . 2_656 ? B1 C1 B1 124.6(10) . 2_656 ? C2 C1 B4 118.4(5) . . ? B2 C1 B4 29.0(6) 2_656 . ? B2 C1 B4 116.6(7) . . ? B3 C1 B4 89.1(9) 2_656 . ? B3 C1 B4 65.9(9) . . ? B1 C1 B4 111.5(8) . . ? B1 C1 B4 36.0(8) 2_656 . ? C2 C1 B4 118.4(5) . 2_656 ? B2 C1 B4 116.6(7) 2_656 2_656 ? B2 C1 B4 29.0(6) . 2_656 ? B3 C1 B4 65.9(9) 2_656 2_656 ? B3 C1 B4 89.1(9) . 2_656 ? B1 C1 B4 36.0(8) . 2_656 ? B1 C1 B4 111.5(8) 2_656 2_656 ? B4 C1 B4 123.1(10) . 2_656 ? C2 C1 B5 119.3(5) . . ? B2 C1 B5 31.0(7) 2_656 . ? B2 C1 B5 114.7(7) . . ? B3 C1 B5 32.3(7) 2_656 . ? B3 C1 B5 114.1(7) . . ? B1 C1 B5 61.5(9) . . ? B1 C1 B5 91.2(9) 2_656 . ? B4 C1 B5 58.5(9) . . ? B4 C1 B5 93.2(8) 2_656 . ? C2 C1 B5 119.3(5) . 2_656 ? B2 C1 B5 114.7(7) 2_656 2_656 ? B2 C1 B5 31.0(7) . 2_656 ? B3 C1 B5 114.1(7) 2_656 2_656 ? B3 C1 B5 32.3(7) . 2_656 ? B1 C1 B5 91.2(9) . 2_656 ? B1 C1 B5 61.5(9) 2_656 2_656 ? B4 C1 B5 93.2(8) . 2_656 ? B4 C1 B5 58.5(9) 2_656 2_656 ? B5 C1 B5 121.3(10) . 2_656 ? O1 C2 O1 129.0(7) 2_656 . ? O1 C2 C1 115.5(3) 2_656 . ? O1 C2 C1 115.5(3) . . ? C4 C3 B10 117.7(7) . . ? C4 C3 B10 117.7(7) . 6_565 ? B10 C3 B10 37.8(14) . 6_565 ? C4 C3 B9 118.6(6) . . ? B10 C3 B9 62.3(9) . . ? B10 C3 B9 95.9(11) 6_565 . ? C4 C3 B9 118.6(6) . 6_565 ? B10 C3 B9 95.9(10) . 6_565 ? B10 C3 B9 62.3(9) 6_565 6_565 ? B9 C3 B9 122.5(12) . 6_565 ? C4 C3 B8 118.6(6) . 6_565 ? B10 C3 B8 122.9(8) . 6_565 ? B10 C3 B8 115.5(8) 6_565 6_565 ? B9 C3 B8 83.0(9) . 6_565 ? B9 C3 B8 65.0(8) 6_565 6_565 ? C4 C3 B8 118.6(6) . . ? B10 C3 B8 115.5(8) . . ? B10 C3 B8 122.9(8) 6_565 . ? B9 C3 B8 65.0(8) . . ? B9 C3 B8 83.0(9) 6_565 . ? B8 C3 B8 19.9(8) 6_565 . ? C4 C3 B6 118.1(7) . 6_565 ? B10 C3 B6 24.3(7) . 6_565 ? B10 C3 B6 61.3(12) 6_565 6_565 ? B9 C3 B6 38.8(9) . 6_565 ? B9 C3 B6 112.8(11) 6_565 6_565 ? B8 C3 B6 112.9(9) 6_565 6_565 ? B8 C3 B6 99.1(8) . 6_565 ? C4 C3 B6 118.1(7) . . ? B10 C3 B6 61.3(12) . . ? B10 C3 B6 24.3(7) 6_565 . ? B9 C3 B6 112.8(11) . . ? B9 C3 B6 38.8(9) 6_565 . ? B8 C3 B6 99.1(8) 6_565 . ? B8 C3 B6 112.9(9) . . ? B6 C3 B6 83.5(14) 6_565 . ? C4 C3 B7 117.7(6) . . ? B10 C3 B7 113.0(9) . . ? B10 C3 B7 83.8(9) 6_565 . ? B9 C3 B7 115.5(9) . . ? B9 C3 B7 23.0(6) 6_565 . ? B8 C3 B7 43.1(8) 6_565 . ? B8 C3 B7 62.3(8) . . ? B6 C3 B7 123.1(9) 6_565 . ? B6 C3 B7 61.3(9) . . ? C4 C3 B7 117.7(6) . 6_565 ? B10 C3 B7 83.8(9) . 6_565 ? B10 C3 B7 113.0(9) 6_565 6_565 ? B9 C3 B7 23.0(6) . 6_565 ? B9 C3 B7 115.5(9) 6_565 6_565 ? B8 C3 B7 62.3(8) 6_565 6_565 ? B8 C3 B7 43.1(8) . 6_565 ? B6 C3 B7 61.3(9) 6_565 6_565 ? B6 C3 B7 123.1(9) . 6_565 ? B7 C3 B7 100.8(14) . 6_565 ? O3 C4 O2 127.4(7) . . ? O3 C4 C3 116.7(6) . . ? O2 C4 C3 115.9(6) . . ? O4 O4 Cu1 81.13(19) 6_565 . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.142 _refine_diff_density_min -0.812 _refine_diff_density_rms 0.140