Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Aldridge, Simon' 'Calder, R. J.' 'Coles, Simon J.' 'Dickinson, A. A.' 'Evans, D.' 'Hursthouse, M.' 'Jones, C.' 'Light, Mark E.' 'Rossin, Andrea' 'Steed, Jon' 'Willcock, David J.' _publ_contact_author_name 'Dr Simon Aldridge' _publ_contact_author_address ; Department of Chemistry Cardiff University PO Box 912 Park Place Cardiff CF10 3TB UK ; _publ_contact_author_email 'ALDRIDGES@CARDIFF.AC.UK' _publ_section_title ; Linking of metal centres through boryl ligands: synthesis, spectroscopic and structural characterisation of symmetrically bridged boryl complexes ; data_001 _database_code_CSD 177260 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H54 O6 Si6' _chemical_formula_weight 607.21 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' 'Si' 'Si' 0.0817 0.0704 '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 18.520(2) _cell_length_b 17.898(2) _cell_length_c 12.451(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.00(2) _cell_angle_gamma 90.00 _cell_volume 4104.3(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.983 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.230 _exptl_absorpt_correction_type difabs _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Nonius CAD4 _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3943 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.18 _reflns_number_total 3817 _reflns_number_gt 2663 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1483P)^2^+4.5842P] 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 3817 _refine_ls_number_parameters 185 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1033 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.2391 _refine_ls_wR_factor_gt 0.2193 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.269 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.05298(9) 0.0000 0.20134(13) 0.0406(5) Uani 1 2 d S . . Si2 Si 0.11998(10) 0.17738(10) 0.45460(13) 0.0721(6) Uani 1 1 d . . . Si3 Si 0.30753(9) 0.0000 -0.16793(15) 0.0465(5) Uani 1 2 d S . . Si4 Si 0.39405(6) 0.18089(7) 0.07931(11) 0.0442(4) Uani 1 1 d . . . O1 O 0.0865(2) 0.0000 0.3314(3) 0.0419(10) Uani 1 2 d S . . O2 O 0.04239(17) 0.13459(17) 0.4159(2) 0.0472(8) Uani 1 1 d . . . O3 O 0.35037(19) 0.0000 -0.0437(3) 0.0345(9) Uani 1 2 d S . . O4 O 0.42500(14) 0.13424(14) -0.0213(2) 0.0350(7) Uani 1 1 d . . . C1 C 0.0421(3) 0.0000 0.4146(4) 0.0356(13) Uani 1 2 d S . . C2 C 0.0214(2) 0.0674(2) 0.4574(3) 0.0380(9) Uani 1 1 d . . . C3 C 0.1342(4) 0.0000 0.1263(6) 0.073(2) Uani 1 2 d S . . H3A H 0.1194 0.0049 0.0504 0.109 Uiso 0.50 1 calc PR . . H3B H 0.1602 -0.0461 0.1394 0.109 Uiso 0.50 1 calc PR . . H3C H 0.1651 0.0411 0.1501 0.109 Uiso 0.50 1 calc PR . . C4 C -0.0035(3) -0.0840(3) 0.1697(4) 0.0630(14) Uani 1 1 d . . . H4A H -0.0234 -0.0824 0.0954 0.094 Uiso 1 1 calc R . . H4B H -0.0423 -0.0852 0.2152 0.094 Uiso 1 1 calc R . . H4C H 0.0259 -0.1280 0.1822 0.094 Uiso 1 1 calc R . . C5 C 0.1669(5) 0.1907(6) 0.3384(8) 0.142(3) Uani 1 1 d U . . H5A H 0.2045 0.1538 0.3376 0.213 Uiso 1 1 calc R . . H5B H 0.1881 0.2397 0.3405 0.213 Uiso 1 1 calc R . . H5C H 0.1335 0.1857 0.2745 0.213 Uiso 1 1 calc R . . C6 C 0.0937(5) 0.2803(5) 0.4790(8) 0.128(3) Uani 1 1 d U . . H6A H 0.1345 0.3060 0.5159 0.191 Uiso 1 1 calc R . . H6B H 0.0538 0.2816 0.5222 0.191 Uiso 1 1 calc R . . H6C H 0.0799 0.3041 0.4109 0.191 Uiso 1 1 calc R . . C7 C 0.1543(6) 0.1443(7) 0.5852(8) 0.160(4) Uani 1 1 d U . . H7A H 0.1697 0.1860 0.6305 0.240 Uiso 1 1 calc R . . H7B H 0.1948 0.1117 0.5788 0.240 Uiso 1 1 calc R . . H7C H 0.1168 0.1174 0.6165 0.240 Uiso 1 1 calc R . . C8 C 0.4245(3) 0.0000 -0.0222(4) 0.0294(11) Uani 1 2 d S . . C9 C 0.46206(19) 0.0672(2) -0.0099(3) 0.0290(8) Uani 1 1 d . . . C10 C 0.3353(4) 0.0830(5) -0.2452(6) 0.113(3) Uani 1 1 d U . . H10A H 0.3187 0.0769 -0.3204 0.169 Uiso 1 1 calc R . . H10B H 0.3873 0.0874 -0.2366 0.169 Uiso 1 1 calc R . . H10C H 0.3142 0.1274 -0.2183 0.169 Uiso 1 1 calc R . . C11 C 0.2119(4) 0.0000 -0.1534(8) 0.092(3) Uani 1 2 d S . . H11A H 0.1849 -0.0004 -0.2235 0.138 Uiso 1 2 calc SR . . H11B H 0.1998 0.0440 -0.1150 0.138 Uiso 0.50 1 calc PR . . H11C H 0.2000 -0.0436 -0.1139 0.138 Uiso 0.50 1 calc PR . . C12 C 0.3647(3) 0.2707(3) 0.0147(6) 0.0734(17) Uani 1 1 d . . . H12A H 0.3428 0.3014 0.0657 0.110 Uiso 1 1 calc R . . H12B H 0.3300 0.2612 -0.0466 0.110 Uiso 1 1 calc R . . H12C H 0.4060 0.2961 -0.0085 0.110 Uiso 1 1 calc R . . C13 C 0.3168(3) 0.1301(3) 0.1293(5) 0.0706(16) Uani 1 1 d . . . H13A H 0.2963 0.1600 0.1825 0.106 Uiso 1 1 calc R . . H13B H 0.3338 0.0836 0.1612 0.106 Uiso 1 1 calc R . . H13C H 0.2805 0.1204 0.0702 0.106 Uiso 1 1 calc R . . C14 C 0.4669(3) 0.1931(3) 0.1913(4) 0.0646(15) Uani 1 1 d . . . H14A H 0.4511 0.2277 0.2430 0.097 Uiso 1 1 calc R . . H14B H 0.5096 0.2123 0.1634 0.097 Uiso 1 1 calc R . . H14C H 0.4777 0.1458 0.2256 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 Si1 0.0447(10) 0.0492(10) 0.0298(8) 0.000 0.0125(7) 0.000 Si2 0.0875(12) 0.0714(11) 0.0574(9) -0.0006(7) 0.0072(8) -0.0397(9) Si3 0.0275(8) 0.0599(12) 0.0503(10) 0.000 -0.0051(7) 0.000 Si4 0.0371(7) 0.0353(7) 0.0615(8) -0.0049(5) 0.0109(6) 0.0078(5) O1 0.037(2) 0.060(3) 0.032(2) 0.000 0.0149(17) 0.000 O2 0.062(2) 0.0430(18) 0.0373(15) 0.0038(13) 0.0077(14) -0.0128(14) O3 0.0214(17) 0.036(2) 0.047(2) 0.000 0.0045(16) 0.000 O4 0.0302(13) 0.0285(14) 0.0462(16) 0.0024(12) 0.0040(12) 0.0039(11) C1 0.035(3) 0.048(3) 0.025(3) 0.000 0.011(2) 0.000 C2 0.038(2) 0.045(2) 0.031(2) 0.0045(18) 0.0045(17) -0.0033(18) C3 0.061(5) 0.117(7) 0.045(4) 0.000 0.026(4) 0.000 C4 0.078(4) 0.064(3) 0.045(3) 0.002(2) 0.000(3) -0.012(3) C5 0.106(4) 0.176(6) 0.151(5) -0.014(4) 0.045(4) -0.069(4) C6 0.152(5) 0.100(5) 0.129(5) -0.024(4) 0.008(4) -0.020(4) C7 0.133(5) 0.169(5) 0.166(5) 0.055(4) -0.041(4) -0.033(4) C8 0.024(2) 0.034(3) 0.031(3) 0.000 0.004(2) 0.000 C9 0.0263(18) 0.0265(19) 0.0343(19) 0.0007(16) 0.0038(14) 0.0041(15) C10 0.114(4) 0.129(4) 0.088(4) 0.037(3) -0.025(3) -0.038(3) C11 0.044(4) 0.159(10) 0.070(6) 0.000 -0.006(4) 0.000 C12 0.068(3) 0.042(3) 0.109(5) -0.005(3) 0.007(3) 0.018(3) C13 0.060(3) 0.065(4) 0.094(4) -0.011(3) 0.038(3) 0.002(3) C14 0.058(3) 0.072(4) 0.064(3) -0.021(3) 0.009(3) 0.014(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 Si1 O1 1.673(4) . ? Si1 C4 1.850(5) 6 ? Si1 C4 1.850(5) . ? Si1 C3 1.852(7) . ? Si2 O2 1.655(3) . ? Si2 C5 1.780(8) . ? Si2 C7 1.784(9) . ? Si2 C6 1.936(9) . ? Si3 O3 1.663(4) . ? Si3 C11 1.799(8) . ? Si3 C10 1.872(7) 6 ? Si3 C10 1.872(7) . ? Si4 O4 1.657(3) . ? Si4 C14 1.848(6) . ? Si4 C12 1.854(5) . ? Si4 C13 1.856(5) . ? O1 C1 1.389(6) . ? O2 C2 1.381(5) . ? O3 C8 1.370(6) . ? O4 C9 1.383(4) . ? C1 C2 1.389(5) . ? C1 C2 1.389(5) 6 ? C2 C2 1.387(8) 2_556 ? C8 C9 1.390(4) . ? C8 C9 1.390(4) 6 ? C9 C9 1.401(7) 2_655 ? 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 Si1 C4 110.51(18) . 6 ? O1 Si1 C4 110.51(18) . . ? C4 Si1 C4 108.7(4) 6 . ? O1 Si1 C3 104.5(3) . . ? C4 Si1 C3 111.3(2) 6 . ? C4 Si1 C3 111.3(2) . . ? O2 Si2 C5 108.0(3) . . ? O2 Si2 C7 109.1(4) . . ? C5 Si2 C7 128.9(6) . . ? O2 Si2 C6 105.1(3) . . ? C5 Si2 C6 98.8(5) . . ? C7 Si2 C6 104.1(5) . . ? O3 Si3 C11 106.6(3) . . ? O3 Si3 C10 110.4(2) . 6 ? C11 Si3 C10 112.2(3) . 6 ? O3 Si3 C10 110.4(2) . . ? C11 Si3 C10 112.2(3) . . ? C10 Si3 C10 105.1(6) 6 . ? O4 Si4 C14 110.31(19) . . ? O4 Si4 C12 102.6(2) . . ? C14 Si4 C12 112.5(3) . . ? O4 Si4 C13 110.3(2) . . ? C14 Si4 C13 109.4(3) . . ? C12 Si4 C13 111.6(3) . . ? C1 O1 Si1 122.2(4) . . ? C2 O2 Si2 124.3(3) . . ? C8 O3 Si3 123.5(3) . . ? C9 O4 Si4 124.5(2) . . ? O1 C1 C2 119.7(2) . . ? O1 C1 C2 119.7(2) . 6 ? C2 C1 C2 120.6(5) . 6 ? O2 C2 C2 119.5(2) . 2_556 ? O2 C2 C1 120.8(3) . . ? C2 C2 C1 119.7(2) 2_556 . ? O3 C8 C9 120.1(2) . . ? O3 C8 C9 120.1(2) . 6 ? C9 C8 C9 119.8(4) . 6 ? O4 C9 C8 120.1(3) . . ? O4 C9 C9 119.74(18) . 2_655 ? C8 C9 C9 120.1(2) . 2_655 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 Si1 O1 C1 60.2(2) 6 . . . ? C4 Si1 O1 C1 -60.2(2) . . . . ? C3 Si1 O1 C1 180.0 . . . . ? C5 Si2 O2 C2 123.0(5) . . . . ? C7 Si2 O2 C2 -21.1(6) . . . . ? C6 Si2 O2 C2 -132.3(4) . . . . ? C11 Si3 O3 C8 180.0 . . . . ? C10 Si3 O3 C8 57.9(3) 6 . . . ? C10 Si3 O3 C8 -57.9(3) . . . . ? C14 Si4 O4 C9 51.0(4) . . . . ? C12 Si4 O4 C9 171.0(3) . . . . ? C13 Si4 O4 C9 -70.0(3) . . . . ? Si1 O1 C1 C2 -91.4(4) . . . . ? Si1 O1 C1 C2 91.4(4) . . . 6 ? Si2 O2 C2 C2 93.8(5) . . . 2_556 ? Si2 O2 C2 C1 -86.6(5) . . . . ? O1 C1 C2 O2 2.2(7) . . . . ? C2 C1 C2 O2 179.3(3) 6 . . . ? O1 C1 C2 C2 -178.2(5) . . . 2_556 ? C2 C1 C2 C2 -1.1(9) 6 . . 2_556 ? Si3 O3 C8 C9 90.9(4) . . . . ? Si3 O3 C8 C9 -90.9(4) . . . 6 ? Si4 O4 C9 C8 92.1(4) . . . . ? Si4 O4 C9 C9 -90.5(5) . . . 2_655 ? O3 C8 C9 O4 -1.3(6) . . . . ? C9 C8 C9 O4 -179.6(3) 6 . . . ? O3 C8 C9 C9 -178.7(5) . . . 2_655 ? C9 C8 C9 C9 3.0(8) 6 . . 2_655 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.18 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.896 _refine_diff_density_min -0.484 _refine_diff_density_rms 0.080 data_226 _database_code_CSD 177261 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H4 B2 O4' _chemical_formula_weight 161.71 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 10.416(2) _cell_length_b 5.2697(11) _cell_length_c 12.231(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 671.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6611 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 30.51 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 328 _exptl_absorpt_coefficient_mu 0.128 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.9687 _exptl_absorpt_correction_T_max 0.9842 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Area Detector' _diffrn_measurement_method 'Phi and Omega scans to fill Ewald Sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6589 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0215 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 27.50 _reflns_number_total 768 _reflns_number_gt 676 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'DENZO, COLLECT' _computing_data_reduction 'DENZO, COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, Pearce 1995)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0705P)^2^+0.2010P] 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 768 _refine_ls_number_parameters 63 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.1065 _refine_ls_wR_factor_gt 0.1007 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _refine_ls_shift/su_max 0.006 _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 O1 O 0.67636(8) 0.03996(16) 0.66256(6) 0.0260(3) Uani 1 1 d . . . O2 O 0.46909(8) 0.28276(16) 0.31618(6) 0.0269(3) Uani 1 1 d . . . B1 B 0.63421(14) -0.1560(3) 0.72902(11) 0.0275(4) Uani 1 1 d . . . C1 C 0.59295(11) 0.0400(2) 0.57436(9) 0.0233(3) Uani 1 1 d . . . C2 C 0.59209(11) 0.2060(2) 0.48674(10) 0.0249(3) Uani 1 1 d . . . C3 C 0.49477(11) 0.1563(2) 0.41282(10) 0.0234(3) Uani 1 1 d . . . H1 H 0.6757(11) -0.198(2) 0.8098(9) 0.014(3) Uiso 1 1 d . . . H2 H 0.6549(14) 0.345(3) 0.4775(12) 0.033(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0250(5) 0.0262(5) 0.0268(5) -0.0010(3) -0.0014(3) -0.0005(3) O2 0.0296(5) 0.0251(5) 0.0259(5) 0.0034(3) 0.0013(3) -0.0008(3) B1 0.0278(7) 0.0275(7) 0.0272(7) 0.0001(5) 0.0016(5) 0.0024(5) C1 0.0220(6) 0.0227(6) 0.0252(6) -0.0021(4) 0.0009(4) 0.0011(4) C2 0.0242(6) 0.0214(6) 0.0290(6) -0.0003(4) 0.0031(4) -0.0014(4) C3 0.0250(6) 0.0205(6) 0.0247(6) 0.0010(4) 0.0040(4) 0.0011(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 B1 1.3857(16) . ? O1 C1 1.3852(13) . ? O2 B1 1.3818(17) 5_656 ? O2 C3 1.3831(14) . ? B1 O2 1.3818(17) 5_656 ? C1 C2 1.3834(16) . ? C1 C3 1.3890(17) 5_656 ? C2 C3 1.3835(17) . ? C3 C1 1.3890(17) 5_656 ? 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 B1 O1 C1 104.97(9) . . ? B1 O2 C3 105.04(10) 5_656 . ? O2 B1 O1 111.86(11) 5_656 . ? O1 C1 C2 127.41(10) . . ? O1 C1 C3 108.93(10) . 5_656 ? C2 C1 C3 123.65(11) . 5_656 ? C3 C2 C1 113.02(11) . . ? C2 C3 O2 127.51(11) . . ? C2 C3 C1 123.32(11) . 5_656 ? O2 C3 C1 109.16(10) . 5_656 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.186 _refine_diff_density_min -0.222 _refine_diff_density_rms 0.051 data_563 _database_code_CSD 177262 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H16 B2 Fe2 O8' _chemical_formula_weight 541.67 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' 'Fe' 'Fe' 0.3463 0.8444 '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 6.4039(13) _cell_length_b 6.8417(14) _cell_length_c 12.547(3) _cell_angle_alpha 83.82(3) _cell_angle_beta 86.64(3) _cell_angle_gamma 77.38(3) _cell_volume 532.97(19) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5916 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 274 _exptl_absorpt_coefficient_mu 1.410 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.5758 _exptl_absorpt_correction_T_max 0.8490 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Area Detector' _diffrn_measurement_method '\\f and \\w scans to fill Ewald Sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8293 _diffrn_reflns_av_R_equivalents 0.0764 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2401 _reflns_number_gt 2304 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'DENZO, COLLECT' _computing_data_reduction 'DENZO, COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, Pearce 1993)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+0.4530P] 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 SHELXL _refine_ls_extinction_coef 0.018(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2401 _refine_ls_number_parameters 156 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0340 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0840 _refine_ls_wR_factor_gt 0.0830 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 C6 C 0.6154(4) 1.0679(3) 0.3477(2) 0.0268(5) Uani 1 1 d . . . H6A H 0.5204 1.0274 0.4061 0.040 Uiso 1 1 calc R . . H6B H 0.5468 1.1989 0.3121 0.040 Uiso 1 1 calc R . . H6C H 0.7507 1.0781 0.3771 0.040 Uiso 1 1 calc R . . C1 C 0.6800(3) 0.7039(3) 0.29197(16) 0.0171(4) Uani 1 1 d . . . H1 H 0.6620 0.6358 0.3609 0.021 Uiso 1 1 calc R . . C2 C 0.7330(3) 0.6113(3) 0.19530(18) 0.0215(4) Uani 1 1 d . . . H2 H 0.7562 0.4713 0.1881 0.026 Uiso 1 1 calc R . . C3 C 0.7453(3) 0.7665(3) 0.11049(17) 0.0238(4) Uani 1 1 d . . . H3 H 0.7785 0.7481 0.0370 0.029 Uiso 1 1 calc R . . C4 C 0.6996(3) 0.9511(3) 0.15560(17) 0.0211(4) Uani 1 1 d . . . H4 H 0.6965 1.0792 0.1172 0.025 Uiso 1 1 calc R . . C5 C 0.6582(3) 0.9155(3) 0.26886(16) 0.0168(4) Uani 1 1 d . . . C7 C 0.3203(3) 0.6892(3) 0.09488(15) 0.0172(4) Uani 1 1 d . . . C8 C 0.2313(3) 1.0301(3) 0.17841(15) 0.0162(4) Uani 1 1 d . . . C9 C 0.0724(3) 0.6609(2) 0.45321(14) 0.0110(3) Uani 1 1 d . . . C10 C 0.1211(3) 0.4784(3) 0.40864(14) 0.0114(3) Uani 1 1 d . . . C11 C 0.0516(3) 0.3079(3) 0.45302(14) 0.0126(3) Uani 1 1 d . . . H11 H 0.0854 0.1831 0.4225 0.015 Uiso 1 1 calc R . . B1 B 0.2651(3) 0.6998(3) 0.30079(16) 0.0122(4) Uani 1 1 d . . . O1 O 0.2465(3) 0.6064(3) 0.03643(13) 0.0281(4) Uani 1 1 d . . . O2 O 0.0963(2) 1.1723(2) 0.17677(13) 0.0265(3) Uani 1 1 d . . . O3 O 0.2402(2) 0.49973(18) 0.31402(10) 0.0133(3) Uani 1 1 d . . . O4 O 0.1601(2) 0.80107(18) 0.38782(10) 0.0132(3) Uani 1 1 d . . . Fe1 Fe 0.43590(4) 0.81261(3) 0.183579(19) 0.01173(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C6 0.0223(10) 0.0251(10) 0.0338(12) -0.0097(9) -0.0089(9) -0.0012(8) C1 0.0116(8) 0.0206(9) 0.0182(9) 0.0025(7) -0.0063(7) -0.0020(7) C2 0.0120(8) 0.0203(9) 0.0303(11) -0.0044(8) -0.0036(8) 0.0022(7) C3 0.0128(9) 0.0384(12) 0.0208(10) -0.0050(9) 0.0039(7) -0.0071(8) C4 0.0172(9) 0.0264(10) 0.0216(10) 0.0043(8) -0.0020(8) -0.0117(8) C5 0.0110(8) 0.0207(9) 0.0191(9) -0.0002(7) -0.0052(7) -0.0040(7) C7 0.0148(8) 0.0210(9) 0.0141(9) -0.0007(7) -0.0001(7) -0.0009(7) C8 0.0165(9) 0.0186(9) 0.0146(9) 0.0021(7) -0.0046(7) -0.0067(7) C9 0.0120(8) 0.0100(8) 0.0114(8) 0.0001(6) -0.0020(6) -0.0033(6) C10 0.0102(7) 0.0129(8) 0.0109(8) -0.0017(6) -0.0016(6) -0.0015(6) C11 0.0148(8) 0.0107(8) 0.0129(8) -0.0031(6) -0.0012(7) -0.0029(6) B1 0.0107(8) 0.0130(9) 0.0124(9) -0.0003(7) -0.0027(7) -0.0014(7) O1 0.0267(8) 0.0361(9) 0.0244(8) -0.0117(7) -0.0046(6) -0.0078(7) O2 0.0224(7) 0.0182(7) 0.0360(9) -0.0010(6) -0.0070(7) 0.0028(6) O3 0.0161(6) 0.0122(6) 0.0114(6) -0.0010(5) 0.0022(5) -0.0034(5) O4 0.0161(6) 0.0107(6) 0.0131(6) 0.0007(5) 0.0013(5) -0.0044(5) Fe1 0.01063(16) 0.01279(17) 0.01134(17) 0.00100(10) -0.00203(10) -0.00220(10) _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 C6 C5 1.486(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C1 C2 1.418(3) . ? C1 C5 1.423(3) . ? C1 Fe1 2.0903(19) . ? C1 H1 0.9500 . ? C2 C3 1.432(3) . ? C2 Fe1 2.093(2) . ? C2 H2 0.9500 . ? C3 C4 1.405(3) . ? C3 Fe1 2.108(2) . ? C3 H3 0.9500 . ? C4 C5 1.435(3) . ? C4 Fe1 2.1050(19) . ? C4 H4 0.9500 . ? C5 Fe1 2.1081(19) . ? C7 O1 1.153(3) . ? C7 Fe1 1.753(2) . ? C8 O2 1.151(3) . ? C8 Fe1 1.753(2) . ? C9 O4 1.386(2) . ? C9 C10 1.388(3) . ? C9 C11 1.390(3) 2_566 ? C10 O3 1.385(2) . ? C10 C11 1.388(2) . ? C11 C9 1.390(3) 2_566 ? C11 H11 0.9500 . ? B1 O3 1.403(2) . ? B1 O4 1.413(2) . ? B1 Fe1 1.973(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 C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C1 C5 108.81(17) . . ? C2 C1 Fe1 70.31(11) . . ? C5 C1 Fe1 70.86(11) . . ? C2 C1 H1 125.6 . . ? C5 C1 H1 125.6 . . ? Fe1 C1 H1 124.8 . . ? C1 C2 C3 107.78(18) . . ? C1 C2 Fe1 70.07(11) . . ? C3 C2 Fe1 70.62(12) . . ? C1 C2 H2 126.1 . . ? C3 C2 H2 126.1 . . ? Fe1 C2 H2 124.8 . . ? C4 C3 C2 107.67(18) . . ? C4 C3 Fe1 70.41(12) . . ? C2 C3 Fe1 69.53(11) . . ? C4 C3 H3 126.2 . . ? C2 C3 H3 126.2 . . ? Fe1 C3 H3 125.5 . . ? C3 C4 C5 109.15(18) . . ? C3 C4 Fe1 70.64(11) . . ? C5 C4 Fe1 70.21(11) . . ? C3 C4 H4 125.4 . . ? C5 C4 H4 125.4 . . ? Fe1 C4 H4 125.3 . . ? C1 C5 C4 106.58(18) . . ? C1 C5 C6 126.61(19) . . ? C4 C5 C6 126.69(19) . . ? C1 C5 Fe1 69.51(11) . . ? C4 C5 Fe1 69.97(11) . . ? C6 C5 Fe1 128.39(14) . . ? O1 C7 Fe1 179.21(18) . . ? O2 C8 Fe1 178.90(18) . . ? O4 C9 C10 109.18(16) . . ? O4 C9 C11 127.31(16) . 2_566 ? C10 C9 C11 123.48(16) . 2_566 ? O3 C10 C11 127.31(16) . . ? O3 C10 C9 109.00(15) . . ? C11 C10 C9 123.65(17) . . ? C10 C11 C9 112.87(17) . 2_566 ? C10 C11 H11 123.6 . . ? C9 C11 H11 123.6 2_566 . ? O3 B1 O4 109.07(15) . . ? O3 B1 Fe1 124.67(14) . . ? O4 B1 Fe1 126.15(13) . . ? C10 O3 B1 106.60(14) . . ? C9 O4 B1 106.15(14) . . ? C7 Fe1 C8 95.56(9) . . ? C7 Fe1 B1 88.05(9) . . ? C8 Fe1 B1 86.91(9) . . ? C7 Fe1 C1 131.04(8) . . ? C8 Fe1 C1 131.12(9) . . ? B1 Fe1 C1 81.69(8) . . ? C7 Fe1 C2 98.08(9) . . ? C8 Fe1 C2 163.83(9) . . ? B1 Fe1 C2 102.15(9) . . ? C1 Fe1 C2 39.62(8) . . ? C7 Fe1 C4 128.58(9) . . ? C8 Fe1 C4 98.48(8) . . ? B1 Fe1 C4 141.71(8) . . ? C1 Fe1 C4 66.21(8) . . ? C2 Fe1 C4 66.11(8) . . ? C7 Fe1 C3 97.20(9) . . ? C8 Fe1 C3 129.56(9) . . ? B1 Fe1 C3 141.98(8) . . ? C1 Fe1 C3 66.51(8) . . ? C2 Fe1 C3 39.85(8) . . ? C4 Fe1 C3 38.96(9) . . ? C7 Fe1 C5 163.13(9) . . ? C8 Fe1 C5 98.51(8) . . ? B1 Fe1 C5 101.91(8) . . ? C1 Fe1 C5 39.63(7) . . ? C2 Fe1 C5 66.71(8) . . ? C4 Fe1 C5 39.82(8) . . ? C3 Fe1 C5 66.58(8) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.672 _refine_diff_density_min -0.644 _refine_diff_density_rms 0.082 data_873 _database_code_CSD 177263 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9.50 H9 B Fe O4' _chemical_formula_weight 253.83 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' 'Fe' 'Fe' 0.3463 0.8444 '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' _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 26.798(2) _cell_length_b 6.0907(6) _cell_length_c 12.6373(15) _cell_angle_alpha 90.00 _cell_angle_beta 108.968(3) _cell_angle_gamma 90.00 _cell_volume 1950.7(3) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1649 _cell_measurement_theta_min 3.22 _cell_measurement_theta_max 25.01 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.729 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 1.534 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8025 _exptl_absorpt_correction_T_max 0.9700 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius Kappa CCD' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean '9.091 pixels mm^1^' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4641 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0740 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 25.01 _reflns_number_total 1649 _reflns_number_gt 1224 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; COLLECT (Hooft, 1998) ; _computing_cell_refinement ; SCALEPACK (Otwinoski and Minor, 1997), COLLECT (Hooft, 1998) ; _computing_data_reduction ; DENZO (Otwinoski and Minor, 1997), COLLECT (Hooft, 1998) MAXUS (Mackay et al., 1998) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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^)+(0.0283P)^2^+3.9239P] 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 1649 _refine_ls_number_parameters 141 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1054 _refine_ls_wR_factor_gt 0.0886 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2007(2) 0.5079(8) 0.0712(4) 0.0431(14) Uani 1 1 d . . . H1 H 0.2081 0.5865 0.0131 0.052 Uiso 1 1 calc R . . C2 C 0.22319(19) 0.3074(8) 0.1175(4) 0.0384(12) Uani 1 1 d . . . H2 H 0.2490 0.2275 0.0968 0.046 Uiso 1 1 calc R . . C3 C 0.20126(18) 0.2457(8) 0.1986(3) 0.0335(11) Uani 1 1 d . . . H3 H 0.2092 0.1158 0.2425 0.040 Uiso 1 1 calc R . . C4 C 0.16535(19) 0.4085(8) 0.2043(4) 0.0369(12) Uani 1 1 d . . . H4 H 0.1447 0.4082 0.2528 0.044 Uiso 1 1 calc R . . C5 C 0.1651(2) 0.5714(8) 0.1263(4) 0.0441(14) Uani 1 1 d . . . H5 H 0.1445 0.7018 0.1129 0.053 Uiso 1 1 calc R . . C6 C 0.14185(17) 0.1594(7) -0.0831(4) 0.0276(11) Uani 1 1 d . . . C7 C 0.09549(19) 0.0915(7) 0.0624(3) 0.0273(10) Uani 1 1 d . . . C9 C 0.04536(17) 0.7545(7) -0.1854(3) 0.0269(10) Uani 1 1 d . . . H9A H 0.0578 0.8387 -0.2389 0.032 Uiso 1 1 calc R . . H9B H 0.0325 0.8606 -0.1407 0.032 Uiso 1 1 calc R . . C10 C 0.0000 0.6045(10) -0.2500 0.0234(14) Uani 1 2 d S . . C11 C -0.01497(16) 0.4656(7) -0.1657(3) 0.0260(10) Uani 1 1 d . . . H11A H -0.0306 0.5607 -0.1212 0.031 Uiso 1 1 calc R . . H11B H -0.0419 0.3567 -0.2057 0.031 Uiso 1 1 calc R . . B1 B 0.0795(2) 0.4387(9) -0.0646(4) 0.0257(12) Uani 1 1 d . . . Fe1 Fe 0.14149(2) 0.27474(10) 0.04208(5) 0.0257(2) Uani 1 1 d . . . O1 O 0.14307(13) 0.0892(5) -0.1668(3) 0.0370(8) Uani 1 1 d . . . O2 O 0.06536(13) -0.0282(5) 0.0782(2) 0.0339(8) Uani 1 1 d . . . O3 O 0.08887(11) 0.6302(5) -0.1116(2) 0.0273(7) Uani 1 1 d . . . O4 O 0.03000(11) 0.3532(5) -0.0919(2) 0.0281(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.055(4) 0.044(3) 0.022(3) 0.002(2) 0.000(3) -0.027(3) C2 0.024(3) 0.052(3) 0.036(3) -0.010(2) 0.006(2) -0.002(2) C3 0.032(3) 0.040(3) 0.021(2) 0.000(2) -0.002(2) -0.005(2) C4 0.032(3) 0.052(3) 0.025(3) -0.019(2) 0.007(2) -0.003(2) C5 0.044(3) 0.031(3) 0.037(3) -0.010(2) -0.014(3) 0.008(2) C6 0.027(3) 0.025(3) 0.030(3) -0.0020(19) 0.008(2) -0.0051(19) C7 0.032(3) 0.028(3) 0.021(2) 0.0025(19) 0.007(2) 0.005(2) C9 0.034(3) 0.019(2) 0.022(2) 0.0032(18) 0.002(2) 0.0008(19) C10 0.028(4) 0.023(4) 0.018(3) 0.000 0.007(3) 0.000 C11 0.022(3) 0.033(3) 0.020(2) 0.0047(18) 0.004(2) 0.0041(19) B1 0.035(3) 0.029(3) 0.016(3) -0.004(2) 0.012(2) 0.001(2) Fe1 0.0267(4) 0.0289(4) 0.0202(4) -0.0011(3) 0.0057(3) 0.0005(3) O1 0.041(2) 0.043(2) 0.0307(19) -0.0131(15) 0.0169(16) -0.0107(16) O2 0.040(2) 0.036(2) 0.0262(18) 0.0029(14) 0.0116(16) -0.0005(16) O3 0.0264(18) 0.0304(19) 0.0213(16) 0.0032(12) 0.0024(14) -0.0024(13) O4 0.0255(18) 0.0328(18) 0.0245(17) 0.0067(12) 0.0060(14) -0.0007(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 C1 C2 1.403(7) . ? C1 C5 1.405(7) . ? C1 Fe1 2.070(5) . ? C2 C3 1.389(7) . ? C2 Fe1 2.094(5) . ? C3 C4 1.400(7) . ? C3 Fe1 2.110(4) . ? C4 C5 1.397(7) . ? C4 Fe1 2.103(4) . ? C5 Fe1 2.088(5) . ? C6 O1 1.151(5) . ? C6 Fe1 1.734(5) . ? C7 O2 1.152(5) . ? C7 Fe1 1.743(5) . ? C9 O3 1.447(5) . ? C9 C10 1.528(5) . ? C10 C11 1.513(5) 2_554 ? C10 C11 1.513(5) . ? C10 C9 1.528(5) 2_554 ? C11 O4 1.436(5) . ? B1 O4 1.360(6) . ? B1 O3 1.369(6) . ? B1 Fe1 2.030(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 107.6(4) . . ? C2 C1 Fe1 71.2(3) . . ? C5 C1 Fe1 70.9(3) . . ? C3 C2 C1 108.4(5) . . ? C3 C2 Fe1 71.3(3) . . ? C1 C2 Fe1 69.4(3) . . ? C2 C3 C4 108.0(4) . . ? C2 C3 Fe1 70.1(3) . . ? C4 C3 Fe1 70.3(3) . . ? C5 C4 C3 108.2(4) . . ? C5 C4 Fe1 69.9(3) . . ? C3 C4 Fe1 70.9(2) . . ? C4 C5 C1 107.8(5) . . ? C4 C5 Fe1 71.1(3) . . ? C1 C5 Fe1 69.6(3) . . ? O1 C6 Fe1 177.6(4) . . ? O2 C7 Fe1 178.5(4) . . ? O3 C9 C10 111.4(3) . . ? C11 C10 C11 112.0(5) 2_554 . ? C11 C10 C9 111.3(2) 2_554 . ? C11 C10 C9 107.7(2) . . ? C11 C10 C9 107.7(2) 2_554 2_554 ? C11 C10 C9 111.3(2) . 2_554 ? C9 C10 C9 106.5(5) . 2_554 ? O4 C11 C10 111.4(3) . . ? O4 B1 O3 121.2(4) . . ? O4 B1 Fe1 120.0(3) . . ? O3 B1 Fe1 118.7(3) . . ? C6 Fe1 C7 95.1(2) . . ? C6 Fe1 B1 80.77(19) . . ? C7 Fe1 B1 87.0(2) . . ? C6 Fe1 C1 102.1(2) . . ? C7 Fe1 C1 161.91(19) . . ? B1 Fe1 C1 101.2(2) . . ? C6 Fe1 C5 136.5(2) . . ? C7 Fe1 C5 126.2(2) . . ? B1 Fe1 C5 87.7(2) . . ? C1 Fe1 C5 39.5(2) . . ? C6 Fe1 C2 98.0(2) . . ? C7 Fe1 C2 132.8(2) . . ? B1 Fe1 C2 139.9(2) . . ? C1 Fe1 C2 39.4(2) . . ? C5 Fe1 C2 65.6(2) . . ? C6 Fe1 C4 163.0(2) . . ? C7 Fe1 C4 96.3(2) . . ? B1 Fe1 C4 112.36(19) . . ? C1 Fe1 C4 65.7(2) . . ? C5 Fe1 C4 38.9(2) . . ? C2 Fe1 C4 65.04(19) . . ? C6 Fe1 C3 126.4(2) . . ? C7 Fe1 C3 99.55(19) . . ? B1 Fe1 C3 150.71(19) . . ? C1 Fe1 C3 65.59(19) . . ? C5 Fe1 C3 65.34(19) . . ? C2 Fe1 C3 38.60(18) . . ? C4 Fe1 C3 38.81(18) . . ? B1 O3 C9 120.1(4) . . ? B1 O4 C11 121.7(4) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.474 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.099 data_sa1 _database_code_CSD 148084 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H12 B2 Fe2 O8' _chemical_formula_weight 513.62 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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 6.4542(3) _cell_length_b 12.2543(4) _cell_length_c 12.4180(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.604(3) _cell_angle_gamma 90.00 _cell_volume 980.22(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.740 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 516 _exptl_absorpt_coefficient_mu 1.528 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.6570 _exptl_absorpt_correction_T_max 0.8032 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 KappaCCD _diffrn_measurement_method '2o phi+omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6704 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2243 _reflns_number_gt 1983 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 1999)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0147P)^2^+0.6970P] 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 SHELXL _refine_ls_extinction_coef 0.0030(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2243 _refine_ls_number_parameters 170 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0605 _refine_ls_wR_factor_gt 0.0582 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 Fe1 Fe 0.12514(4) 0.789984(19) 0.674843(18) 0.01364(10) Uani 1 1 d . . . O1 O 0.47936(17) 0.88863(10) 0.81029(9) 0.0157(3) Uani 1 1 d . . . C1 C 0.5110(3) 0.94734(13) 0.90562(12) 0.0137(3) Uani 1 1 d . . . B1 B 0.2668(3) 0.86281(15) 0.80039(15) 0.0148(4) Uani 1 1 d . . . O2 O 0.17062(17) 0.90341(10) 0.89064(9) 0.0159(3) Uani 1 1 d . . . C2 C 0.3244(2) 0.95675(13) 0.95408(13) 0.0135(3) Uani 1 1 d . . . O3 O -0.0629(2) 0.64397(12) 0.82532(11) 0.0342(4) Uani 1 1 d . . . C3 C 0.3033(3) 1.01020(14) 1.05074(13) 0.0160(3) Uani 1 1 d . . . H3 H 0.180(4) 1.0161(18) 1.0830(17) 0.033(6) Uiso 1 1 d . . . O4 O 0.4961(2) 0.65821(11) 0.66435(11) 0.0293(3) Uani 1 1 d . . . C4 C 0.0596(3) 0.95285(15) 0.63459(14) 0.0211(4) Uani 1 1 d . . . H4 H 0.093(3) 1.0136(18) 0.6782(16) 0.023(5) Uiso 1 1 d . . . C5 C 0.1828(3) 0.90545(15) 0.55668(14) 0.0204(4) Uani 1 1 d . . . H5 H 0.315(3) 0.9279(17) 0.5412(16) 0.023(5) Uiso 1 1 d . . . C6 C 0.0694(3) 0.81685(15) 0.50733(13) 0.0206(4) Uani 1 1 d . . . H6 H 0.114(3) 0.7676(19) 0.4538(18) 0.032(6) Uiso 1 1 d . . . C7 C -0.1216(3) 0.80913(16) 0.55588(14) 0.0211(4) Uani 1 1 d . . . H7 H -0.223(3) 0.7594(18) 0.5403(16) 0.023(5) Uiso 1 1 d . . . C8 C -0.1272(3) 0.89296(16) 0.63539(14) 0.0219(4) Uani 1 1 d . . . H8 H -0.234(3) 0.9043(17) 0.6791(18) 0.029(6) Uiso 1 1 d . . . C9 C 0.0089(3) 0.70169(15) 0.76492(14) 0.0212(4) Uani 1 1 d . . . C10 C 0.3478(3) 0.70937(14) 0.66775(14) 0.0190(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01480(15) 0.01382(15) 0.01247(14) -0.00021(9) 0.00221(9) -0.00051(9) O1 0.0136(6) 0.0201(6) 0.0138(5) -0.0045(5) 0.0034(4) -0.0010(5) C1 0.0159(8) 0.0142(8) 0.0113(7) -0.0008(6) 0.0028(6) 0.0018(6) B1 0.0152(9) 0.0139(9) 0.0154(9) 0.0023(7) 0.0023(7) 0.0010(7) O2 0.0121(6) 0.0203(6) 0.0153(6) -0.0034(5) 0.0014(4) -0.0012(5) C2 0.0116(8) 0.0142(8) 0.0146(7) 0.0006(6) 0.0012(6) -0.0006(6) O3 0.0380(9) 0.0363(8) 0.0293(8) 0.0101(6) 0.0097(6) -0.0105(7) C3 0.0131(8) 0.0197(9) 0.0156(8) -0.0004(7) 0.0045(6) 0.0008(7) O4 0.0241(7) 0.0242(7) 0.0400(8) -0.0029(6) 0.0057(6) 0.0073(6) C4 0.0322(11) 0.0143(9) 0.0161(8) -0.0004(7) -0.0038(7) 0.0024(7) C5 0.0233(10) 0.0197(9) 0.0182(8) 0.0052(7) 0.0023(7) -0.0025(7) C6 0.0295(10) 0.0204(9) 0.0119(8) -0.0008(7) 0.0017(7) 0.0014(8) C7 0.0200(9) 0.0240(9) 0.0186(9) 0.0021(7) -0.0045(7) -0.0028(8) C8 0.0204(9) 0.0282(10) 0.0172(8) 0.0022(7) 0.0014(7) 0.0076(8) C9 0.0214(9) 0.0223(10) 0.0200(9) -0.0012(7) 0.0015(7) -0.0012(7) C10 0.0247(10) 0.0154(8) 0.0172(8) -0.0019(7) 0.0038(7) -0.0048(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C10 1.7507(19) . ? Fe1 C9 1.7580(19) . ? Fe1 B1 1.9708(19) . ? Fe1 C5 2.0887(18) . ? Fe1 C8 2.0938(18) . ? Fe1 C4 2.0942(18) . ? Fe1 C6 2.1145(17) . ? Fe1 C7 2.1160(18) . ? O1 C1 1.3894(19) . ? O1 B1 1.406(2) . ? C1 C2 1.385(2) . ? C1 C3 1.385(2) 3_677 ? B1 O2 1.406(2) . ? O2 C2 1.3909(19) . ? C2 C3 1.382(2) . ? O3 C9 1.149(2) . ? C3 C1 1.385(2) 3_677 ? O4 C10 1.147(2) . ? C4 C8 1.412(3) . ? C4 C5 1.415(3) . ? C5 C6 1.426(3) . ? C6 C7 1.409(3) . ? C7 C8 1.427(3) . ? 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 C10 Fe1 C9 93.97(8) . . ? C10 Fe1 B1 87.35(8) . . ? C9 Fe1 B1 88.32(8) . . ? C10 Fe1 C5 99.43(8) . . ? C9 Fe1 C5 165.02(8) . . ? B1 Fe1 C5 98.90(7) . . ? C10 Fe1 C8 163.17(8) . . ? C9 Fe1 C8 99.38(8) . . ? B1 Fe1 C8 103.15(8) . . ? C5 Fe1 C8 66.28(8) . . ? C10 Fe1 C4 132.84(8) . . ? C9 Fe1 C4 130.58(8) . . ? B1 Fe1 C4 80.44(7) . . ? C5 Fe1 C4 39.55(7) . . ? C8 Fe1 C4 39.40(8) . . ? C10 Fe1 C6 97.34(8) . . ? C9 Fe1 C6 131.97(8) . . ? B1 Fe1 C6 138.55(8) . . ? C5 Fe1 C6 39.66(7) . . ? C8 Fe1 C6 66.06(7) . . ? C4 Fe1 C6 66.26(7) . . ? C10 Fe1 C7 127.70(8) . . ? C9 Fe1 C7 100.36(8) . . ? B1 Fe1 C7 142.51(8) . . ? C5 Fe1 C7 66.05(7) . . ? C8 Fe1 C7 39.62(7) . . ? C4 Fe1 C7 66.16(7) . . ? C6 Fe1 C7 38.91(7) . . ? C1 O1 B1 106.35(13) . . ? C2 C1 C3 123.61(15) . 3_677 ? C2 C1 O1 109.15(14) . . ? C3 C1 O1 127.23(15) 3_677 . ? O2 B1 O1 109.15(14) . . ? O2 B1 Fe1 125.79(13) . . ? O1 B1 Fe1 124.94(12) . . ? C2 O2 B1 106.42(13) . . ? C3 C2 C1 123.57(15) . . ? C3 C2 O2 127.52(15) . . ? C1 C2 O2 108.90(14) . . ? C2 C3 C1 112.81(15) . 3_677 ? C8 C4 C5 107.95(16) . . ? C8 C4 Fe1 70.28(10) . . ? C5 C4 Fe1 70.01(10) . . ? C4 C5 C6 108.11(17) . . ? C4 C5 Fe1 70.43(10) . . ? C6 C5 Fe1 71.14(10) . . ? C7 C6 C5 107.85(16) . . ? C7 C6 Fe1 70.60(10) . . ? C5 C6 Fe1 69.19(10) . . ? C6 C7 C8 107.97(17) . . ? C6 C7 Fe1 70.49(10) . . ? C8 C7 Fe1 69.35(10) . . ? C4 C8 C7 108.10(16) . . ? C4 C8 Fe1 70.31(10) . . ? C7 C8 Fe1 71.03(11) . . ? O3 C9 Fe1 178.40(17) . . ? O4 C10 Fe1 178.52(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag B1 O1 C1 C2 0.60(18) . . . . ? B1 O1 C1 C3 179.70(17) . . . 3_677 ? C1 O1 B1 O2 -1.39(18) . . . . ? C1 O1 B1 Fe1 174.84(12) . . . . ? C10 Fe1 B1 O2 -146.00(16) . . . . ? C9 Fe1 B1 O2 -51.95(16) . . . . ? C5 Fe1 B1 O2 114.87(15) . . . . ? C8 Fe1 B1 O2 47.29(16) . . . . ? C4 Fe1 B1 O2 79.73(15) . . . . ? C6 Fe1 B1 O2 115.89(15) . . . . ? C7 Fe1 B1 O2 53.0(2) . . . . ? C10 Fe1 B1 O1 38.39(15) . . . . ? C9 Fe1 B1 O1 132.44(16) . . . . ? C5 Fe1 B1 O1 -60.75(16) . . . . ? C8 Fe1 B1 O1 -128.32(15) . . . . ? C4 Fe1 B1 O1 -95.88(15) . . . . ? C6 Fe1 B1 O1 -59.7(2) . . . . ? C7 Fe1 B1 O1 -122.64(16) . . . . ? O1 B1 O2 C2 1.63(17) . . . . ? Fe1 B1 O2 C2 -174.56(13) . . . . ? C3 C1 C2 C3 0.5(3) 3_677 . . . ? O1 C1 C2 C3 179.63(15) . . . . ? C3 C1 C2 O2 -178.73(15) 3_677 . . . ? O1 C1 C2 O2 0.41(18) . . . . ? B1 O2 C2 C3 179.57(17) . . . . ? B1 O2 C2 C1 -1.25(17) . . . . ? C1 C2 C3 C1 -0.4(3) . . . 3_677 ? O2 C2 C3 C1 178.63(15) . . . 3_677 ? C10 Fe1 C4 C8 158.07(11) . . . . ? C9 Fe1 C4 C8 -45.20(14) . . . . ? B1 Fe1 C4 C8 -124.64(11) . . . . ? C5 Fe1 C4 C8 118.60(15) . . . . ? C6 Fe1 C4 C8 80.62(11) . . . . ? C7 Fe1 C4 C8 37.93(10) . . . . ? C10 Fe1 C4 C5 39.46(15) . . . . ? C9 Fe1 C4 C5 -163.81(12) . . . . ? B1 Fe1 C4 C5 116.76(12) . . . . ? C8 Fe1 C4 C5 -118.60(15) . . . . ? C6 Fe1 C4 C5 -37.99(11) . . . . ? C7 Fe1 C4 C5 -80.68(12) . . . . ? C8 C4 C5 C6 1.2(2) . . . . ? Fe1 C4 C5 C6 61.50(12) . . . . ? C8 C4 C5 Fe1 -60.32(12) . . . . ? C10 Fe1 C5 C4 -151.81(11) . . . . ? C9 Fe1 C5 C4 55.0(3) . . . . ? B1 Fe1 C5 C4 -63.03(12) . . . . ? C8 Fe1 C5 C4 37.50(11) . . . . ? C6 Fe1 C5 C4 118.03(16) . . . . ? C7 Fe1 C5 C4 80.99(12) . . . . ? C10 Fe1 C5 C6 90.16(12) . . . . ? C9 Fe1 C5 C6 -63.0(3) . . . . ? B1 Fe1 C5 C6 178.93(11) . . . . ? C8 Fe1 C5 C6 -80.54(12) . . . . ? C4 Fe1 C5 C6 -118.03(16) . . . . ? C7 Fe1 C5 C6 -37.04(11) . . . . ? C4 C5 C6 C7 -0.8(2) . . . . ? Fe1 C5 C6 C7 60.29(12) . . . . ? C4 C5 C6 Fe1 -61.05(12) . . . . ? C10 Fe1 C6 C7 145.29(12) . . . . ? C9 Fe1 C6 C7 43.18(15) . . . . ? B1 Fe1 C6 C7 -120.37(13) . . . . ? C5 Fe1 C6 C7 -118.78(16) . . . . ? C8 Fe1 C6 C7 -37.65(11) . . . . ? C4 Fe1 C6 C7 -80.90(12) . . . . ? C10 Fe1 C6 C5 -95.93(12) . . . . ? C9 Fe1 C6 C5 161.96(12) . . . . ? B1 Fe1 C6 C5 -1.59(17) . . . . ? C8 Fe1 C6 C5 81.13(12) . . . . ? C4 Fe1 C6 C5 37.88(11) . . . . ? C7 Fe1 C6 C5 118.78(16) . . . . ? C5 C6 C7 C8 0.1(2) . . . . ? Fe1 C6 C7 C8 59.45(12) . . . . ? C5 C6 C7 Fe1 -59.40(12) . . . . ? C10 Fe1 C7 C6 -45.54(14) . . . . ? C9 Fe1 C7 C6 -148.86(12) . . . . ? B1 Fe1 C7 C6 110.22(14) . . . . ? C5 Fe1 C7 C6 37.75(11) . . . . ? C8 Fe1 C7 C6 118.91(16) . . . . ? C4 Fe1 C7 C6 81.18(12) . . . . ? C10 Fe1 C7 C8 -164.45(11) . . . . ? C9 Fe1 C7 C8 92.23(12) . . . . ? B1 Fe1 C7 C8 -8.68(18) . . . . ? C5 Fe1 C7 C8 -81.16(12) . . . . ? C4 Fe1 C7 C8 -37.72(11) . . . . ? C6 Fe1 C7 C8 -118.91(16) . . . . ? C5 C4 C8 C7 -1.2(2) . . . . ? Fe1 C4 C8 C7 -61.30(12) . . . . ? C5 C4 C8 Fe1 60.15(12) . . . . ? C6 C7 C8 C4 0.7(2) . . . . ? Fe1 C7 C8 C4 60.85(12) . . . . ? C6 C7 C8 Fe1 -60.16(13) . . . . ? C10 Fe1 C8 C4 -71.1(3) . . . . ? C9 Fe1 C8 C4 146.89(11) . . . . ? B1 Fe1 C8 C4 56.43(12) . . . . ? C5 Fe1 C8 C4 -37.64(10) . . . . ? C6 Fe1 C8 C4 -81.17(11) . . . . ? C7 Fe1 C8 C4 -118.16(15) . . . . ? C10 Fe1 C8 C7 47.1(3) . . . . ? C9 Fe1 C8 C7 -94.95(12) . . . . ? B1 Fe1 C8 C7 174.58(11) . . . . ? C5 Fe1 C8 C7 80.52(12) . . . . ? C4 Fe1 C8 C7 118.16(15) . . . . ? C6 Fe1 C8 C7 36.98(11) . . . . ? C10 Fe1 C9 O3 50(6) . . . . ? B1 Fe1 C9 O3 -37(6) . . . . ? C5 Fe1 C9 O3 -156(6) . . . . ? C8 Fe1 C9 O3 -140(6) . . . . ? C4 Fe1 C9 O3 -113(6) . . . . ? C6 Fe1 C9 O3 154(6) . . . . ? C7 Fe1 C9 O3 180(100) . . . . ? C9 Fe1 C10 O4 -109(7) . . . . ? B1 Fe1 C10 O4 -21(7) . . . . ? C5 Fe1 C10 O4 78(7) . . . . ? C8 Fe1 C10 O4 108(7) . . . . ? C4 Fe1 C10 O4 53(7) . . . . ? C6 Fe1 C10 O4 118(7) . . . . ? C7 Fe1 C10 O4 144(7) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.331 _refine_diff_density_min -0.255 _refine_diff_density_rms 0.060 data_sa2 _database_code_CSD 142393 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H2 B2 Cl2 O4' _chemical_formula_weight 230.60 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' 'Cl' 'Cl' 0.1484 0.1585 '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 4.4108(9) _cell_length_b 6.7612(14) _cell_length_c 7.5147(15) _cell_angle_alpha 105.64(3) _cell_angle_beta 103.88(3) _cell_angle_gamma 91.38(3) _cell_volume 208.56(7) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.836 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 114 _exptl_absorpt_coefficient_mu 0.753 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.7528 _exptl_absorpt_correction_T_max 0.9633 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '2o phi + omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 1535 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0717 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.49 _reflns_number_total 949 _reflns_number_gt 735 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 1999)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.1080P] 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 SHELXL _refine_ls_extinction_coef 0.022(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 949 _refine_ls_number_parameters 69 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.0854 _refine_ls_wR_factor_gt 0.0779 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.17722(15) 0.81111(10) 0.61471(9) 0.0251(2) Uani 1 1 d . . . O1 O 0.6977(4) 0.8166(3) 0.9023(2) 0.0185(4) Uani 1 1 d . . . O2 O 0.4762(4) 0.4919(3) 0.7184(2) 0.0185(4) Uani 1 1 d . . . C2 C 0.7407(5) 0.4745(4) 0.8571(3) 0.0150(5) Uani 1 1 d . . . C1 C 0.8753(5) 0.6696(4) 0.9668(3) 0.0149(5) Uani 1 1 d . . . C3 C 0.8567(6) 0.2950(4) 0.8841(3) 0.0173(5) Uani 1 1 d . . . B1 B 0.4610(6) 0.7014(5) 0.7518(4) 0.0192(6) Uani 1 1 d . . . H3 H 0.767(6) 0.164(4) 0.812(4) 0.017(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0248(4) 0.0309(4) 0.0215(4) 0.0112(3) 0.0044(2) 0.0118(3) O1 0.0192(9) 0.0171(9) 0.0209(10) 0.0080(7) 0.0047(7) 0.0065(7) O2 0.0155(8) 0.0188(9) 0.0197(10) 0.0065(7) 0.0003(7) 0.0026(7) C2 0.0095(10) 0.0212(13) 0.0150(12) 0.0074(10) 0.0018(9) 0.0018(9) C1 0.0153(11) 0.0148(12) 0.0186(13) 0.0092(10) 0.0064(9) 0.0057(9) C3 0.0184(12) 0.0144(13) 0.0178(13) 0.0035(10) 0.0037(10) -0.0001(10) B1 0.0179(13) 0.0248(15) 0.0188(15) 0.0075(12) 0.0100(11) 0.0058(11) _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 Cl1 B1 1.737(3) . ? O1 B1 1.377(3) . ? O1 C1 1.397(3) . ? O2 B1 1.377(3) . ? O2 C2 1.396(3) . ? C2 C3 1.375(3) . ? C2 C1 1.384(3) . ? C1 C3 1.384(3) 2_767 ? C3 C1 1.384(3) 2_767 ? 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 B1 O1 C1 104.15(19) . . ? B1 O2 C2 104.1(2) . . ? C3 C2 C1 123.9(2) . . ? C3 C2 O2 126.8(2) . . ? C1 C2 O2 109.3(2) . . ? C2 C1 C3 123.5(2) . 2_767 ? C2 C1 O1 109.1(2) . . ? C3 C1 O1 127.4(2) 2_767 . ? C2 C3 C1 112.6(2) . 2_767 ? O2 B1 O1 113.4(2) . . ? O2 B1 Cl1 123.6(2) . . ? O1 B1 Cl1 123.0(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag B1 O2 C2 C3 179.9(3) . . . . ? B1 O2 C2 C1 -0.3(3) . . . . ? C3 C2 C1 C3 0.3(4) . . . 2_767 ? O2 C2 C1 C3 -179.5(2) . . . 2_767 ? C3 C2 C1 O1 -179.5(2) . . . . ? O2 C2 C1 O1 0.7(3) . . . . ? B1 O1 C1 C2 -0.7(3) . . . . ? B1 O1 C1 C3 179.4(2) . . . 2_767 ? C1 C2 C3 C1 -0.3(4) . . . 2_767 ? O2 C2 C3 C1 179.5(2) . . . 2_767 ? C2 O2 B1 O1 -0.2(3) . . . . ? C2 O2 B1 Cl1 178.44(19) . . . . ? C1 O1 B1 O2 0.6(3) . . . . ? C1 O1 B1 Cl1 -178.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.341 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.085