# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Merle Arrowsmith' 'Terrance J. Hadlington' 'Michael S. Hill' 'Gabriele Kociok-Kohn' _publ_contact_author_email M.S.Hill@bath.ac.uk _publ_contact_author_name 'Michael S. Hill' data_h11msh8 _database_code_depnum_ccdc_archive 'CCDC 863862' #TrackingRef 'h11msh8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C61 H75 B Mg N2 O4' _chemical_formula_sum 'C61 H75 B Mg N2 O4' _chemical_formula_weight 935.35 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' Mg Mg 0.0486 0.0363 '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 orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 19.2649(2) _cell_length_b 20.4622(3) _cell_length_c 26.9490(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10623.4(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 196133 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 25.350 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.170 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4032 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9563 _exptl_absorpt_correction_T_max 0.9679 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 Kappa CCD' _diffrn_measurement_method '709 1.0 degree images with \f and \w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 115166 _diffrn_reflns_av_R_equivalents 0.0914 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 25.39 _reflns_number_total 9691 _reflns_number_gt 6837 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Institut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0538P)^2^+8.7366P] 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 9691 _refine_ls_number_parameters 636 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0893 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1465 _refine_ls_wR_factor_gt 0.1281 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg Mg 0.56791(4) 0.23881(4) 0.38613(3) 0.02408(18) Uani 1 1 d . . . B B 0.66166(11) 0.33402(10) 0.37531(8) 0.0118(4) Uani 1 1 d . . . N1 N 0.53986(10) 0.15762(9) 0.42637(7) 0.0261(4) Uani 1 1 d . . . N2 N 0.48729(10) 0.23273(9) 0.33705(7) 0.0299(5) Uani 1 1 d . . . O1 O 0.65643(8) 0.26404(7) 0.35418(6) 0.0272(4) Uani 1 1 d . . . O2 O 0.73152(8) 0.33891(7) 0.39369(6) 0.0306(4) Uani 1 1 d . . . O3 O 0.60354(7) 0.32219(7) 0.41708(5) 0.0234(3) Uani 1 1 d . . . O4 O 0.63665(9) 0.38492(8) 0.34402(7) 0.0373(4) Uani 1 1 d . . . C1 C 0.47209(12) 0.14212(11) 0.42719(9) 0.0307(5) Uani 1 1 d . . . C2 C 0.44379(14) 0.09333(13) 0.46458(10) 0.0410(7) Uani 1 1 d . . . H2A H 0.4817 0.0777 0.4857 0.062 Uiso 1 1 calc R . . H2B H 0.4230 0.0563 0.4470 0.062 Uiso 1 1 calc R . . H2C H 0.4084 0.1146 0.4852 0.062 Uiso 1 1 calc R . . C3 C 0.42205(13) 0.16767(12) 0.39522(10) 0.0350(6) Uani 1 1 d . . . H3 H 0.3755 0.1596 0.4051 0.042 Uiso 1 1 calc R . . C4 C 0.42886(13) 0.20326(12) 0.35100(9) 0.0349(6) Uani 1 1 d . . . C5 C 0.36453(15) 0.20453(16) 0.31860(12) 0.0548(8) Uani 1 1 d . . . H5A H 0.3313 0.2363 0.3319 0.082 Uiso 1 1 calc R . . H5B H 0.3432 0.1610 0.3182 0.082 Uiso 1 1 calc R . . H5C H 0.3774 0.2171 0.2847 0.082 Uiso 1 1 calc R . . C6 C 0.58635(12) 0.11490(11) 0.45324(9) 0.0275(5) Uani 1 1 d . . . C7 C 0.61504(12) 0.13481(11) 0.49898(9) 0.0280(5) Uani 1 1 d . . . C8 C 0.59757(13) 0.20078(12) 0.52205(9) 0.0312(5) Uani 1 1 d . . . H8 H 0.5961 0.2336 0.4946 0.037 Uiso 1 1 calc R . . C9 C 0.52604(14) 0.20038(13) 0.54677(10) 0.0423(7) Uani 1 1 d . . . H9A H 0.4903 0.1918 0.5217 0.063 Uiso 1 1 calc R . . H9B H 0.5174 0.2429 0.5623 0.063 Uiso 1 1 calc R . . H9C H 0.5246 0.1661 0.5721 0.063 Uiso 1 1 calc R . . C10 C 0.65156(15) 0.22427(13) 0.55972(10) 0.0421(7) Uani 1 1 d . . . H10A H 0.6497 0.1965 0.5893 0.063 Uiso 1 1 calc R . . H10B H 0.6416 0.2696 0.5690 0.063 Uiso 1 1 calc R . . H10C H 0.6980 0.2218 0.5449 0.063 Uiso 1 1 calc R . . C11 C 0.65871(13) 0.09163(12) 0.52383(10) 0.0352(6) Uani 1 1 d . . . H11 H 0.6782 0.1043 0.5547 0.042 Uiso 1 1 calc R . . C12 C 0.67435(13) 0.03106(12) 0.50479(10) 0.0389(6) Uani 1 1 d . . . H12 H 0.7043 0.0024 0.5225 0.047 Uiso 1 1 calc R . . C13 C 0.64646(14) 0.01210(12) 0.46006(10) 0.0392(6) Uani 1 1 d . . . H13 H 0.6576 -0.0298 0.4472 0.047 Uiso 1 1 calc R . . C14 C 0.60210(13) 0.05294(11) 0.43303(9) 0.0326(6) Uani 1 1 d . . . C15 C 0.57292(15) 0.02851(13) 0.38382(10) 0.0421(7) Uani 1 1 d . . . H15 H 0.5457 0.0647 0.3682 0.050 Uiso 1 1 calc R . . C16 C 0.63041(18) 0.00860(14) 0.34831(12) 0.0548(8) Uani 1 1 d . . . H16A H 0.6635 0.0447 0.3448 0.082 Uiso 1 1 calc R . . H16B H 0.6104 -0.0018 0.3158 0.082 Uiso 1 1 calc R . . H16C H 0.6544 -0.0299 0.3614 0.082 Uiso 1 1 calc R . . C17 C 0.52451(17) -0.03049(16) 0.39107(13) 0.0614(9) Uani 1 1 d . . . H17A H 0.5518 -0.0684 0.4017 0.092 Uiso 1 1 calc R . . H17B H 0.5011 -0.0405 0.3597 0.092 Uiso 1 1 calc R . . H17C H 0.4897 -0.0201 0.4164 0.092 Uiso 1 1 calc R . . C18 C 0.49162(13) 0.25734(12) 0.28685(9) 0.0342(6) Uani 1 1 d . . . C19 C 0.52696(14) 0.21879(13) 0.25167(9) 0.0408(6) Uani 1 1 d . . . C20 C 0.55671(16) 0.15232(14) 0.26553(10) 0.0497(7) Uani 1 1 d . . . H20 H 0.5755 0.1559 0.3000 0.060 Uiso 1 1 calc R . . C21 C 0.6161(2) 0.12986(18) 0.23210(12) 0.0717(11) Uani 1 1 d . . . H21A H 0.6378 0.0908 0.2464 0.108 Uiso 1 1 calc R . . H21B H 0.6507 0.1648 0.2294 0.108 Uiso 1 1 calc R . . H21C H 0.5979 0.1195 0.1991 0.108 Uiso 1 1 calc R . . C22 C 0.4992(2) 0.09992(15) 0.26630(13) 0.0695(10) Uani 1 1 d . . . H22A H 0.4754 0.0993 0.2342 0.104 Uiso 1 1 calc R . . H22B H 0.4657 0.1102 0.2926 0.104 Uiso 1 1 calc R . . H22C H 0.5198 0.0570 0.2727 0.104 Uiso 1 1 calc R . . C23 C 0.53066(16) 0.24104(15) 0.20316(10) 0.0512(8) Uani 1 1 d . . . H23 H 0.5544 0.2157 0.1790 0.061 Uiso 1 1 calc R . . C24 C 0.50058(17) 0.29907(16) 0.18945(11) 0.0553(8) Uani 1 1 d . . . H24 H 0.5023 0.3130 0.1558 0.066 Uiso 1 1 calc R . . C25 C 0.46801(15) 0.33707(15) 0.22443(10) 0.0470(7) Uani 1 1 d . . . H25 H 0.4483 0.3776 0.2145 0.056 Uiso 1 1 calc R . . C26 C 0.46285(13) 0.31838(13) 0.27371(9) 0.0367(6) Uani 1 1 d . . . C27 C 0.42725(13) 0.36387(12) 0.31022(10) 0.0380(6) Uani 1 1 d . . . H27 H 0.4270 0.3426 0.3436 0.046 Uiso 1 1 calc R . . C28 C 0.35217(15) 0.37901(16) 0.29532(13) 0.0577(8) Uani 1 1 d . . . H28A H 0.3518 0.4024 0.2636 0.087 Uiso 1 1 calc R . . H28B H 0.3305 0.4063 0.3209 0.087 Uiso 1 1 calc R . . H28C H 0.3262 0.3381 0.2920 0.087 Uiso 1 1 calc R . . C29 C 0.46832(15) 0.42811(14) 0.31380(11) 0.0487(7) Uani 1 1 d . . . H29A H 0.5149 0.4191 0.3268 0.073 Uiso 1 1 calc R . . H29B H 0.4441 0.4583 0.3361 0.073 Uiso 1 1 calc R . . H29C H 0.4722 0.4478 0.2808 0.073 Uiso 1 1 calc R . . C30 C 0.72775(12) 0.24157(12) 0.34761(9) 0.0315(5) Uani 1 1 d . . . C31 C 0.72879(14) 0.16781(12) 0.34949(11) 0.0413(6) Uani 1 1 d . . . H31A H 0.7046 0.1529 0.3794 0.062 Uiso 1 1 calc R . . H31B H 0.7770 0.1525 0.3502 0.062 Uiso 1 1 calc R . . H31C H 0.7054 0.1502 0.3201 0.062 Uiso 1 1 calc R . . C32 C 0.75198(15) 0.26598(14) 0.29682(10) 0.0445(7) Uani 1 1 d . . . H32A H 0.7199 0.2505 0.2712 0.067 Uiso 1 1 calc R . . H32B H 0.7987 0.2493 0.2900 0.067 Uiso 1 1 calc R . . H32C H 0.7528 0.3139 0.2968 0.067 Uiso 1 1 calc R . . C33 C 0.76569(12) 0.27645(12) 0.39120(9) 0.0318(6) Uani 1 1 d . . . C34 C 0.75588(13) 0.24069(12) 0.44062(9) 0.0350(6) Uani 1 1 d . . . H34A H 0.7738 0.2679 0.4677 0.053 Uiso 1 1 calc R . . H34B H 0.7812 0.1992 0.4398 0.053 Uiso 1 1 calc R . . H34C H 0.7064 0.2322 0.4460 0.053 Uiso 1 1 calc R . . C35 C 0.84231(13) 0.28851(15) 0.38213(12) 0.0497(7) Uani 1 1 d . . . H35A H 0.8480 0.3171 0.3533 0.074 Uiso 1 1 calc R . . H35B H 0.8657 0.2468 0.3759 0.074 Uiso 1 1 calc R . . H35C H 0.8628 0.3094 0.4114 0.074 Uiso 1 1 calc R . . C36 C 0.57509(11) 0.37690(10) 0.44407(8) 0.0248(5) Uani 1 1 d . . . H36 H 0.5877 0.4174 0.4254 0.030 Uiso 1 1 calc R . . C37 C 0.49662(12) 0.37302(11) 0.44527(8) 0.0269(5) Uani 1 1 d . . . C38 C 0.46244(12) 0.31442(12) 0.45382(9) 0.0310(5) Uani 1 1 d . . . H38 H 0.4886 0.2757 0.4593 0.037 Uiso 1 1 calc R . . C39 C 0.39033(13) 0.31156(14) 0.45452(10) 0.0414(6) Uani 1 1 d . . . H39 H 0.3675 0.2711 0.4600 0.050 Uiso 1 1 calc R . . C40 C 0.35219(14) 0.36773(15) 0.44717(11) 0.0485(7) Uani 1 1 d . . . H40 H 0.3029 0.3659 0.4471 0.058 Uiso 1 1 calc R . . C41 C 0.38556(14) 0.42647(15) 0.43987(11) 0.0499(8) Uani 1 1 d . . . H41 H 0.3593 0.4653 0.4354 0.060 Uiso 1 1 calc R . . C42 C 0.45741(13) 0.42901(13) 0.43900(10) 0.0379(6) Uani 1 1 d . . . H42 H 0.4800 0.4697 0.4340 0.046 Uiso 1 1 calc R . . C43 C 0.60766(12) 0.38248(10) 0.49589(8) 0.0262(5) Uani 1 1 d . . . C44 C 0.56771(13) 0.39332(12) 0.53797(9) 0.0338(6) Uani 1 1 d . . . H44 H 0.5186 0.3948 0.5352 0.041 Uiso 1 1 calc R . . C45 C 0.59850(15) 0.40207(13) 0.58401(10) 0.0417(6) Uani 1 1 d . . . H45 H 0.5704 0.4096 0.6124 0.050 Uiso 1 1 calc R . . C46 C 0.66999(14) 0.39986(13) 0.58883(10) 0.0405(6) Uani 1 1 d . . . H46 H 0.6911 0.4054 0.6204 0.049 Uiso 1 1 calc R . . C47 C 0.70996(13) 0.38957(12) 0.54733(10) 0.0348(6) Uani 1 1 d . . . H47 H 0.7591 0.3880 0.5503 0.042 Uiso 1 1 calc R . . C48 C 0.67946(12) 0.38141(11) 0.50105(9) 0.0299(5) Uani 1 1 d . . . H48 H 0.7079 0.3750 0.4727 0.036 Uiso 1 1 calc R . . C49 C 0.67979(14) 0.43737(13) 0.32911(10) 0.0391(6) Uani 1 1 d . . . H49 H 0.7287 0.4262 0.3381 0.047 Uiso 1 1 calc R . . C50 C 0.65880(13) 0.49780(13) 0.35849(10) 0.0372(6) Uani 1 1 d . . . C51 C 0.60715(14) 0.53974(13) 0.34240(11) 0.0453(7) Uani 1 1 d . . . H51 H 0.5864 0.5332 0.3108 0.054 Uiso 1 1 calc R . . C52 C 0.58545(15) 0.59128(14) 0.37197(12) 0.0500(7) Uani 1 1 d . . . H52 H 0.5499 0.6198 0.3605 0.060 Uiso 1 1 calc R . . C53 C 0.61510(15) 0.60141(14) 0.41784(11) 0.0484(7) Uani 1 1 d . . . H53 H 0.6000 0.6366 0.4381 0.058 Uiso 1 1 calc R . . C54 C 0.66672(15) 0.56010(14) 0.43406(11) 0.0468(7) Uani 1 1 d . . . H54 H 0.6875 0.5667 0.4656 0.056 Uiso 1 1 calc R . . C55 C 0.68816(14) 0.50908(13) 0.40436(10) 0.0413(6) Uani 1 1 d . . . H55 H 0.7240 0.4810 0.4158 0.050 Uiso 1 1 calc R . . C56 C 0.67670(14) 0.44806(14) 0.27360(10) 0.0419(7) Uani 1 1 d . . . C57 C 0.71136(16) 0.50077(15) 0.25317(12) 0.0530(8) Uani 1 1 d . . . H57 H 0.7364 0.5294 0.2744 0.064 Uiso 1 1 calc R . . C58 C 0.71059(18) 0.51280(17) 0.20290(12) 0.0612(9) Uani 1 1 d . . . H58 H 0.7347 0.5495 0.1898 0.073 Uiso 1 1 calc R . . C59 C 0.67461(18) 0.47128(18) 0.17150(12) 0.0635(9) Uani 1 1 d . . . H59 H 0.6733 0.4794 0.1368 0.076 Uiso 1 1 calc R . . C60 C 0.64090(18) 0.41813(18) 0.19132(12) 0.0622(9) Uani 1 1 d . . . H60 H 0.6168 0.3890 0.1700 0.075 Uiso 1 1 calc R . . C61 C 0.64157(16) 0.40652(15) 0.24195(11) 0.0496(7) Uani 1 1 d . . . H61 H 0.6177 0.3697 0.2550 0.060 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 Mg 0.0257(4) 0.0260(4) 0.0205(4) 0.0012(3) -0.0009(3) -0.0034(3) B 0.0127(11) 0.0114(10) 0.0113(11) -0.0002(8) -0.0025(8) 0.0011(8) N1 0.0279(11) 0.0258(10) 0.0246(11) 0.0022(8) 0.0001(8) -0.0028(8) N2 0.0351(11) 0.0320(11) 0.0225(10) 0.0011(8) -0.0048(9) -0.0039(9) O1 0.0264(8) 0.0316(9) 0.0237(9) -0.0015(7) 0.0037(7) -0.0007(7) O2 0.0349(9) 0.0266(9) 0.0303(9) 0.0025(7) -0.0010(7) -0.0035(7) O3 0.0239(8) 0.0242(8) 0.0220(8) -0.0018(6) 0.0037(6) -0.0008(6) O4 0.0331(10) 0.0377(10) 0.0412(10) 0.0003(8) -0.0043(8) -0.0017(8) C1 0.0334(14) 0.0291(13) 0.0297(13) -0.0006(10) 0.0019(10) -0.0068(10) C2 0.0383(15) 0.0425(15) 0.0424(16) 0.0099(12) 0.0033(12) -0.0108(12) C3 0.0270(13) 0.0405(14) 0.0377(15) 0.0029(11) -0.0017(11) -0.0088(11) C4 0.0331(14) 0.0378(14) 0.0337(14) 0.0002(11) -0.0094(11) -0.0073(11) C5 0.0465(17) 0.063(2) 0.0552(19) 0.0137(15) -0.0212(15) -0.0180(15) C6 0.0275(13) 0.0270(12) 0.0281(13) 0.0066(10) 0.0038(10) -0.0050(10) C7 0.0284(13) 0.0271(12) 0.0285(13) 0.0051(10) 0.0025(10) -0.0050(9) C8 0.0362(14) 0.0331(13) 0.0242(13) 0.0044(10) -0.0005(10) -0.0050(11) C9 0.0494(17) 0.0448(16) 0.0326(15) -0.0011(12) 0.0115(13) -0.0044(13) C10 0.0565(18) 0.0357(14) 0.0340(15) 0.0028(11) -0.0107(13) -0.0053(12) C11 0.0350(14) 0.0366(14) 0.0340(14) 0.0092(11) -0.0037(11) -0.0080(11) C12 0.0379(15) 0.0325(14) 0.0463(17) 0.0161(12) -0.0028(13) -0.0001(11) C13 0.0456(16) 0.0248(12) 0.0471(17) 0.0053(12) 0.0043(13) -0.0001(11) C14 0.0367(14) 0.0269(13) 0.0342(14) 0.0047(10) 0.0029(11) -0.0050(10) C15 0.0557(18) 0.0314(14) 0.0391(16) -0.0038(12) -0.0041(13) 0.0027(12) C16 0.073(2) 0.0409(16) 0.0504(19) -0.0091(14) 0.0104(16) -0.0110(15) C17 0.058(2) 0.060(2) 0.066(2) -0.0198(17) -0.0028(17) -0.0173(16) C18 0.0371(14) 0.0439(15) 0.0216(12) 0.0020(11) -0.0082(10) -0.0084(12) C19 0.0506(17) 0.0472(16) 0.0247(13) -0.0046(12) -0.0084(12) -0.0044(13) C20 0.067(2) 0.0525(17) 0.0299(15) -0.0125(13) -0.0091(14) 0.0071(15) C21 0.094(3) 0.081(2) 0.0393(18) -0.0193(17) -0.0014(18) 0.028(2) C22 0.099(3) 0.0470(19) 0.062(2) -0.0134(16) -0.027(2) -0.0075(18) C23 0.061(2) 0.066(2) 0.0269(15) -0.0064(14) -0.0041(13) -0.0027(16) C24 0.069(2) 0.072(2) 0.0244(15) 0.0106(14) -0.0069(14) -0.0081(17) C25 0.0535(18) 0.0543(18) 0.0333(16) 0.0123(13) -0.0104(13) -0.0020(14) C26 0.0359(14) 0.0441(15) 0.0301(14) 0.0048(11) -0.0091(11) -0.0051(12) C27 0.0374(15) 0.0405(14) 0.0360(15) 0.0072(12) -0.0082(12) -0.0019(12) C28 0.0416(17) 0.068(2) 0.064(2) 0.0022(17) -0.0128(15) 0.0047(15) C29 0.0532(18) 0.0453(16) 0.0476(18) 0.0058(13) -0.0069(14) -0.0036(13) C30 0.0288(13) 0.0350(13) 0.0306(13) 0.0010(11) 0.0085(10) 0.0030(10) C31 0.0427(16) 0.0373(15) 0.0439(16) -0.0039(12) 0.0039(12) 0.0053(12) C32 0.0460(16) 0.0542(17) 0.0334(15) 0.0009(13) 0.0173(13) 0.0026(13) C33 0.0278(13) 0.0325(13) 0.0352(14) 0.0023(11) 0.0021(11) 0.0012(10) C34 0.0366(14) 0.0329(13) 0.0356(14) 0.0063(11) -0.0026(11) 0.0032(11) C35 0.0300(15) 0.0568(18) 0.062(2) 0.0055(15) 0.0045(13) -0.0024(13) C36 0.0273(12) 0.0234(11) 0.0238(12) -0.0021(9) 0.0031(9) -0.0002(9) C37 0.0277(13) 0.0325(13) 0.0206(12) -0.0022(10) 0.0011(9) 0.0011(10) C38 0.0264(13) 0.0381(14) 0.0283(13) -0.0019(10) 0.0039(10) 0.0011(10) C39 0.0309(14) 0.0493(16) 0.0440(16) -0.0092(13) 0.0061(12) -0.0075(12) C40 0.0246(14) 0.064(2) 0.0571(19) -0.0065(15) 0.0006(13) 0.0065(13) C41 0.0371(16) 0.0551(19) 0.0575(19) 0.0006(15) 0.0022(14) 0.0163(14) C42 0.0351(15) 0.0354(14) 0.0433(16) -0.0006(12) 0.0026(12) 0.0044(11) C43 0.0322(13) 0.0215(11) 0.0250(12) -0.0009(9) -0.0003(10) -0.0009(9) C44 0.0336(14) 0.0384(14) 0.0295(14) -0.0060(11) 0.0022(11) -0.0002(11) C45 0.0491(17) 0.0472(16) 0.0288(14) -0.0103(12) 0.0033(12) -0.0003(13) C46 0.0505(17) 0.0390(15) 0.0319(15) -0.0050(12) -0.0106(13) -0.0071(12) C47 0.0321(14) 0.0333(13) 0.0390(15) 0.0020(11) -0.0081(12) -0.0059(11) C48 0.0303(13) 0.0295(12) 0.0298(13) 0.0015(10) 0.0006(10) -0.0026(10) C49 0.0343(14) 0.0400(15) 0.0431(16) -0.0004(12) -0.0030(12) 0.0022(12) C50 0.0331(14) 0.0403(15) 0.0382(15) -0.0024(12) 0.0000(12) -0.0027(11) C51 0.0427(17) 0.0455(16) 0.0477(17) -0.0073(13) -0.0060(13) 0.0034(13) C52 0.0401(17) 0.0485(17) 0.061(2) -0.0083(15) 0.0021(14) 0.0035(13) C53 0.0427(17) 0.0482(17) 0.0544(19) -0.0153(14) 0.0130(14) -0.0077(13) C54 0.0511(18) 0.0519(17) 0.0375(16) -0.0057(13) 0.0021(13) -0.0098(14) C55 0.0420(16) 0.0411(15) 0.0408(16) 0.0002(12) -0.0014(13) -0.0045(12) C56 0.0376(15) 0.0478(16) 0.0405(16) -0.0057(13) 0.0030(12) 0.0010(12) C57 0.0554(19) 0.0592(19) 0.0442(18) -0.0047(15) 0.0024(14) 0.0002(15) C58 0.069(2) 0.066(2) 0.049(2) 0.0049(16) 0.0072(17) -0.0014(17) C59 0.067(2) 0.085(3) 0.0380(18) 0.0017(17) 0.0009(16) 0.0135(19) C60 0.065(2) 0.078(2) 0.0443(19) -0.0044(17) -0.0038(16) -0.0041(18) C61 0.0533(18) 0.0561(18) 0.0395(17) -0.0050(14) -0.0026(14) -0.0001(14) _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 Mg O1 1.9789(16) . ? Mg O3 2.0194(16) . ? Mg N2 2.044(2) . ? Mg N1 2.0561(19) . ? Mg B 2.673(2) . ? B O4 1.424(3) . ? B O2 1.438(3) . ? B O1 1.544(3) . ? B O3 1.606(3) . ? N1 C1 1.344(3) . ? N1 C6 1.446(3) . ? N2 C4 1.331(3) . ? N2 C18 1.446(3) . ? O1 C30 1.460(3) . ? O2 C33 1.439(3) . ? O3 C36 1.443(3) . ? O4 C49 1.416(3) . ? C1 C3 1.395(3) . ? C1 C2 1.520(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.403(3) . ? C3 H3 0.9500 . ? C4 C5 1.516(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.411(3) . ? C6 C14 1.413(3) . ? C7 C11 1.392(3) . ? C7 C8 1.524(3) . ? C8 C9 1.531(3) . ? C8 C10 1.531(3) . ? C8 H8 1.0000 . ? 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 C12 1.375(4) . ? C11 H11 0.9500 . ? C12 C13 1.376(4) . ? C12 H12 0.9500 . ? C13 C14 1.400(4) . ? C13 H13 0.9500 . ? C14 C15 1.525(4) . ? C15 C16 1.519(4) . ? C15 C17 1.538(4) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.409(4) . ? C18 C26 1.412(4) . ? C19 C23 1.386(4) . ? C19 C20 1.522(4) . ? C20 C21 1.527(4) . ? C20 C22 1.543(4) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.372(4) . ? C23 H23 0.9500 . ? C24 C25 1.374(4) . ? C24 H24 0.9500 . ? C25 C26 1.385(4) . ? C25 H25 0.9500 . ? C26 C27 1.518(4) . ? C27 C28 1.533(4) . ? C27 C29 1.537(4) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.510(3) . ? C30 C32 1.530(3) . ? C30 C33 1.557(3) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C35 1.517(3) . ? C33 C34 1.531(3) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.514(3) . ? C36 C43 1.535(3) . ? C36 H36 1.0000 . ? C37 C42 1.383(3) . ? C37 C38 1.387(3) . ? C38 C39 1.391(3) . ? C38 H38 0.9500 . ? C39 C40 1.379(4) . ? C39 H39 0.9500 . ? C40 C41 1.377(4) . ? C40 H40 0.9500 . ? C41 C42 1.385(4) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.388(3) . ? C43 C48 1.390(3) . ? C44 C45 1.387(4) . ? C44 H44 0.9500 . ? C45 C46 1.384(4) . ? C45 H45 0.9500 . ? C46 C47 1.374(4) . ? C46 H46 0.9500 . ? C47 C48 1.389(3) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C56 1.513(4) . ? C49 C50 1.523(4) . ? C49 H49 1.0000 . ? C50 C55 1.379(4) . ? C50 C51 1.384(4) . ? C51 C52 1.386(4) . ? C51 H51 0.9500 . ? C52 C53 1.378(4) . ? C52 H52 0.9500 . ? C53 C54 1.376(4) . ? C53 H53 0.9500 . ? C54 C55 1.379(4) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C56 C61 1.381(4) . ? C56 C57 1.383(4) . ? C57 C58 1.377(4) . ? C57 H57 0.9500 . ? C58 C59 1.385(5) . ? C58 H58 0.9500 . ? C59 C60 1.375(5) . ? C59 H59 0.9500 . ? C60 C61 1.385(4) . ? C60 H60 0.9500 . ? C61 H61 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 O1 Mg O3 70.51(6) . . ? O1 Mg N2 112.90(8) . . ? O3 Mg N2 125.24(8) . . ? O1 Mg N1 131.82(8) . . ? O3 Mg N1 123.65(8) . . ? N2 Mg N1 95.31(8) . . ? O1 Mg B 34.91(6) . . ? O3 Mg B 36.82(6) . . ? N2 Mg B 119.16(8) . . ? N1 Mg B 145.50(8) . . ? O4 B O2 118.02(17) . . ? O4 B O1 115.95(16) . . ? O2 B O1 104.64(15) . . ? O4 B O3 106.83(16) . . ? O2 B O3 114.94(16) . . ? O1 B O3 94.20(13) . . ? O4 B Mg 111.66(13) . . ? O2 B Mg 130.23(13) . . ? O1 B Mg 47.17(8) . . ? O3 B Mg 48.89(8) . . ? C1 N1 C6 116.80(18) . . ? C1 N1 Mg 117.04(15) . . ? C6 N1 Mg 126.15(14) . . ? C4 N2 C18 118.1(2) . . ? C4 N2 Mg 119.17(16) . . ? C18 N2 Mg 122.72(15) . . ? C30 O1 B 105.98(15) . . ? C30 O1 Mg 141.43(14) . . ? B O1 Mg 97.92(11) . . ? B O2 C33 110.50(16) . . ? C36 O3 B 120.06(15) . . ? C36 O3 Mg 137.26(13) . . ? B O3 Mg 94.29(10) . . ? C49 O4 B 121.60(18) . . ? N1 C1 C3 125.0(2) . . ? N1 C1 C2 121.0(2) . . ? C3 C1 C2 114.1(2) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 C4 130.9(2) . . ? C1 C3 H3 114.6 . . ? C4 C3 H3 114.6 . . ? N2 C4 C3 123.7(2) . . ? N2 C4 C5 121.4(2) . . ? C3 C4 C5 114.9(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C14 120.8(2) . . ? C7 C6 N1 120.4(2) . . ? C14 C6 N1 118.9(2) . . ? C11 C7 C6 118.3(2) . . ? C11 C7 C8 120.0(2) . . ? C6 C7 C8 121.7(2) . . ? C7 C8 C9 111.8(2) . . ? C7 C8 C10 113.5(2) . . ? C9 C8 C10 109.0(2) . . ? C7 C8 H8 107.4 . . ? C9 C8 H8 107.4 . . ? C10 C8 H8 107.4 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C7 121.7(2) . . ? C12 C11 H11 119.2 . . ? C7 C11 H11 119.2 . . ? C11 C12 C13 119.7(2) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C12 C13 C14 121.7(2) . . ? C12 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C13 C14 C6 117.8(2) . . ? C13 C14 C15 118.8(2) . . ? C6 C14 C15 123.4(2) . . ? C16 C15 C14 111.5(2) . . ? C16 C15 C17 108.2(2) . . ? C14 C15 C17 111.7(2) . . ? C16 C15 H15 108.4 . . ? C14 C15 H15 108.4 . . ? C17 C15 H15 108.4 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C26 121.1(2) . . ? C19 C18 N2 117.6(2) . . ? C26 C18 N2 121.3(2) . . ? C23 C19 C18 118.4(3) . . ? C23 C19 C20 120.4(3) . . ? C18 C19 C20 121.1(2) . . ? C19 C20 C21 114.0(3) . . ? C19 C20 C22 110.7(3) . . ? C21 C20 C22 109.7(3) . . ? C19 C20 H20 107.4 . . ? C21 C20 H20 107.4 . . ? C22 C20 H20 107.4 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C19 121.1(3) . . ? C24 C23 H23 119.4 . . ? C19 C23 H23 119.4 . . ? C23 C24 C25 119.9(3) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C24 C25 C26 122.3(3) . . ? C24 C25 H25 118.9 . . ? C26 C25 H25 118.9 . . ? C25 C26 C18 117.2(3) . . ? C25 C26 C27 119.0(2) . . ? C18 C26 C27 123.9(2) . . ? C26 C27 C28 112.4(2) . . ? C26 C27 C29 109.4(2) . . ? C28 C27 C29 109.2(2) . . ? C26 C27 H27 108.6 . . ? C28 C27 H27 108.6 . . ? C29 C27 H27 108.6 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O1 C30 C31 108.85(19) . . ? O1 C30 C32 107.04(19) . . ? C31 C30 C32 110.6(2) . . ? O1 C30 C33 101.88(17) . . ? C31 C30 C33 115.3(2) . . ? C32 C30 C33 112.5(2) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O2 C33 C35 108.0(2) . . ? O2 C33 C34 109.11(19) . . ? C35 C33 C34 109.8(2) . . ? O2 C33 C30 103.16(18) . . ? C35 C33 C30 114.2(2) . . ? C34 C33 C30 112.3(2) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O3 C36 C37 110.44(17) . . ? O3 C36 C43 111.14(17) . . ? C37 C36 C43 113.11(18) . . ? O3 C36 H36 107.3 . . ? C37 C36 H36 107.3 . . ? C43 C36 H36 107.3 . . ? C42 C37 C38 118.5(2) . . ? C42 C37 C36 120.0(2) . . ? C38 C37 C36 121.5(2) . . ? C37 C38 C39 120.9(2) . . ? C37 C38 H38 119.6 . . ? C39 C38 H38 119.6 . . ? C40 C39 C38 119.7(3) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C41 C40 C39 120.0(2) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C42 120.1(3) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C37 C42 C41 120.8(2) . . ? C37 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C44 C43 C48 118.2(2) . . ? C44 C43 C36 121.9(2) . . ? C48 C43 C36 119.8(2) . . ? C45 C44 C43 120.9(2) . . ? C45 C44 H44 119.5 . . ? C43 C44 H44 119.5 . . ? C46 C45 C44 120.4(2) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C47 C46 C45 119.1(2) . . ? C47 C46 H46 120.5 . . ? C45 C46 H46 120.5 . . ? C46 C47 C48 120.8(2) . . ? C46 C47 H47 119.6 . . ? C48 C47 H47 119.6 . . ? C47 C48 C43 120.6(2) . . ? C47 C48 H48 119.7 . . ? C43 C48 H48 119.7 . . ? O4 C49 C56 111.5(2) . . ? O4 C49 C50 108.2(2) . . ? C56 C49 C50 112.7(2) . . ? O4 C49 H49 108.1 . . ? C56 C49 H49 108.1 . . ? C50 C49 H49 108.1 . . ? C55 C50 C51 118.2(3) . . ? C55 C50 C49 119.5(2) . . ? C51 C50 C49 122.1(2) . . ? C50 C51 C52 120.6(3) . . ? C50 C51 H51 119.7 . . ? C52 C51 H51 119.7 . . ? C53 C52 C51 120.3(3) . . ? C53 C52 H52 119.8 . . ? C51 C52 H52 119.8 . . ? C54 C53 C52 119.5(3) . . ? C54 C53 H53 120.3 . . ? C52 C53 H53 120.3 . . ? C53 C54 C55 119.8(3) . . ? C53 C54 H54 120.1 . . ? C55 C54 H54 120.1 . . ? C54 C55 C50 121.6(3) . . ? C54 C55 H55 119.2 . . ? C50 C55 H55 119.2 . . ? C61 C56 C57 118.1(3) . . ? C61 C56 C49 122.7(3) . . ? C57 C56 C49 119.2(3) . . ? C58 C57 C56 121.7(3) . . ? C58 C57 H57 119.1 . . ? C56 C57 H57 119.1 . . ? C57 C58 C59 119.8(3) . . ? C57 C58 H58 120.1 . . ? C59 C58 H58 120.1 . . ? C60 C59 C58 119.0(3) . . ? C60 C59 H59 120.5 . . ? C58 C59 H59 120.5 . . ? C59 C60 C61 120.9(3) . . ? C59 C60 H60 119.5 . . ? C61 C60 H60 119.5 . . ? C56 C61 C60 120.5(3) . . ? C56 C61 H61 119.8 . . ? C60 C61 H61 119.8 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.276 _refine_diff_density_min -0.310 _refine_diff_density_rms 0.048 # Attachment 'k11msh12.cif' data_k11msh12 _database_code_depnum_ccdc_archive 'CCDC 863863' #TrackingRef 'k11msh12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H36 B2 O6' _chemical_formula_sum 'C26 H36 B2 O6' _chemical_formula_weight 466.17 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 monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' 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 8.2719(2) _cell_length_b 9.9302(2) _cell_length_c 15.8441(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.8300(10) _cell_angle_gamma 90.00 _cell_volume 1268.97(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 22947 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.60 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.220 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 500 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9516 _exptl_absorpt_correction_T_max 0.9516 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 Kappa CCD' _diffrn_measurement_method '298 2.0 degree images with \f and \w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 21410 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0175 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.53 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2878 _reflns_number_gt 2576 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Institut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0537P)^2^+0.5950P] 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 2878 _refine_ls_number_parameters 158 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1233 _refine_ls_wR_factor_gt 0.1190 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 B B 0.07330(18) 0.32206(15) 0.37428(9) 0.0253(3) Uani 1 1 d . . . O1 O -0.03848(13) 0.36742(10) 0.30336(6) 0.0326(2) Uani 1 1 d . . . O2 O 0.13296(12) 0.19606(10) 0.36734(6) 0.0319(2) Uani 1 1 d . . . O3 O 0.12902(11) 0.39572(9) 0.44820(6) 0.0267(2) Uani 1 1 d . . . C1 C -0.08103(18) 0.25137(13) 0.24523(8) 0.0292(3) Uani 1 1 d . . . C2 C -0.2430(2) 0.19490(19) 0.26042(11) 0.0438(4) Uani 1 1 d . . . H2A H -0.2281 0.1679 0.3212 0.066 Uiso 1 1 calc R . . H2B H -0.2758 0.1164 0.2230 0.066 Uiso 1 1 calc R . . H2C H -0.3295 0.2640 0.2469 0.066 Uiso 1 1 calc R . . C3 C -0.1040(3) 0.30014(17) 0.15258(10) 0.0454(4) Uani 1 1 d . . . H3A H -0.1933 0.3670 0.1404 0.068 Uiso 1 1 calc R . . H3B H -0.1327 0.2237 0.1129 0.068 Uiso 1 1 calc R . . H3C H -0.0007 0.3412 0.1445 0.068 Uiso 1 1 calc R . . C4 C 0.07039(19) 0.15511(15) 0.27756(9) 0.0323(3) Uani 1 1 d . . . C5 C 0.0233(3) 0.00715(17) 0.27851(12) 0.0544(5) Uani 1 1 d . . . H5A H 0.1232 -0.0468 0.3000 0.082 Uiso 1 1 calc R . . H5B H -0.0293 -0.0217 0.2197 0.082 Uiso 1 1 calc R . . H5C H -0.0543 -0.0054 0.3164 0.082 Uiso 1 1 calc R . . C6 C 0.2103(3) 0.1741(3) 0.23158(13) 0.0597(5) Uani 1 1 d . . . H6A H 0.2364 0.2702 0.2297 0.090 Uiso 1 1 calc R . . H6B H 0.1768 0.1392 0.1724 0.090 Uiso 1 1 calc R . . H6C H 0.3085 0.1252 0.2627 0.090 Uiso 1 1 calc R . . C7 C 0.04582(15) 0.51606(12) 0.46368(8) 0.0231(3) Uani 1 1 d . . . H7 H -0.0368 0.5418 0.4099 0.028 Uiso 1 1 calc R . . C8 C 0.17081(16) 0.62884(13) 0.48870(8) 0.0235(3) Uani 1 1 d . . . C9 C 0.33421(16) 0.60090(14) 0.52991(9) 0.0279(3) Uani 1 1 d . . . H9 H 0.3682 0.5103 0.5421 0.033 Uiso 1 1 calc R . . C10 C 0.44811(18) 0.70491(16) 0.55329(9) 0.0333(3) Uani 1 1 d . . . H10 H 0.5595 0.6848 0.5811 0.040 Uiso 1 1 calc R . . C11 C 0.40007(19) 0.83722(15) 0.53632(9) 0.0352(3) Uani 1 1 d . . . H11 H 0.4781 0.9079 0.5528 0.042 Uiso 1 1 calc R . . C12 C 0.2377(2) 0.86664(15) 0.49518(9) 0.0359(3) Uani 1 1 d . . . H12 H 0.2044 0.9575 0.4832 0.043 Uiso 1 1 calc R . . C13 C 0.12323(18) 0.76234(14) 0.47143(9) 0.0304(3) Uani 1 1 d . . . H13 H 0.0121 0.7826 0.4433 0.036 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 B 0.0249(7) 0.0261(7) 0.0263(7) -0.0013(5) 0.0085(5) -0.0025(5) O1 0.0453(6) 0.0234(5) 0.0272(5) -0.0055(4) 0.0042(4) 0.0032(4) O2 0.0346(5) 0.0293(5) 0.0299(5) -0.0081(4) 0.0034(4) 0.0035(4) O3 0.0252(4) 0.0257(5) 0.0286(5) -0.0074(4) 0.0043(4) 0.0020(3) C1 0.0410(7) 0.0241(6) 0.0230(6) -0.0059(5) 0.0079(5) -0.0021(5) C2 0.0400(8) 0.0506(10) 0.0401(8) -0.0072(7) 0.0069(6) -0.0090(7) C3 0.0710(12) 0.0384(8) 0.0261(7) 0.0011(6) 0.0091(7) 0.0015(8) C4 0.0410(8) 0.0306(7) 0.0256(6) -0.0071(5) 0.0085(5) 0.0004(6) C5 0.0814(14) 0.0280(8) 0.0453(9) -0.0046(7) -0.0043(9) 0.0035(8) C6 0.0520(11) 0.0838(15) 0.0508(11) -0.0118(10) 0.0278(9) 0.0066(10) C7 0.0244(6) 0.0223(6) 0.0224(6) -0.0046(5) 0.0050(5) 0.0002(5) C8 0.0285(6) 0.0236(6) 0.0196(5) -0.0034(4) 0.0082(5) -0.0039(5) C9 0.0276(6) 0.0279(6) 0.0292(6) -0.0022(5) 0.0086(5) -0.0025(5) C10 0.0276(7) 0.0393(8) 0.0341(7) -0.0047(6) 0.0094(5) -0.0084(6) C11 0.0423(8) 0.0342(7) 0.0325(7) -0.0054(6) 0.0153(6) -0.0170(6) C12 0.0512(9) 0.0243(7) 0.0337(7) 0.0004(5) 0.0124(6) -0.0057(6) C13 0.0356(7) 0.0266(7) 0.0281(6) -0.0003(5) 0.0053(5) -0.0007(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 B O2 1.3584(18) . ? B O1 1.3634(18) . ? B O3 1.3709(17) . ? O1 C1 1.4684(15) . ? O2 C4 1.4595(16) . ? O3 C7 1.4272(15) . ? C1 C3 1.5172(19) . ? C1 C2 1.520(2) . ? C1 C4 1.568(2) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C6 1.510(2) . ? C4 C5 1.521(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.5160(17) . ? C7 C7 1.546(2) 3_566 ? C7 H7 1.0000 . ? C8 C9 1.3922(19) . ? C8 C13 1.3926(19) . ? C9 C10 1.3917(19) . ? C9 H9 0.9500 . ? C10 C11 1.382(2) . ? C10 H10 0.9500 . ? C11 C12 1.388(2) . ? C11 H11 0.9500 . ? C12 C13 1.397(2) . ? C12 H12 0.9500 . ? C13 H13 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 O2 B O1 115.45(12) . . ? O2 B O3 120.08(12) . . ? O1 B O3 124.45(12) . . ? B O1 C1 106.37(10) . . ? B O2 C4 106.19(11) . . ? B O3 C7 120.67(10) . . ? O1 C1 C3 108.51(11) . . ? O1 C1 C2 106.69(11) . . ? C3 C1 C2 110.22(13) . . ? O1 C1 C4 102.16(10) . . ? C3 C1 C4 115.45(12) . . ? C2 C1 C4 113.05(12) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O2 C4 C6 106.95(13) . . ? O2 C4 C5 107.20(12) . . ? C6 C4 C5 110.53(15) . . ? O2 C4 C1 103.48(10) . . ? C6 C4 C1 114.11(14) . . ? C5 C4 C1 113.85(13) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 C8 109.67(10) . . ? O3 C7 C7 106.86(12) . 3_566 ? C8 C7 C7 112.12(12) . 3_566 ? O3 C7 H7 109.4 . . ? C8 C7 H7 109.4 . . ? C7 C7 H7 109.4 3_566 . ? C9 C8 C13 118.98(12) . . ? C9 C8 C7 120.68(12) . . ? C13 C8 C7 120.35(12) . . ? C10 C9 C8 120.42(13) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C11 C10 C9 120.36(14) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 119.88(13) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C11 C12 C13 119.85(14) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C8 C13 C12 120.51(13) . . ? C8 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.421 _refine_diff_density_min -0.263 _refine_diff_density_rms 0.041