# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Sjoerd Harder' _publ_contact_author_email s.harder@rug.nl loop_ _publ_author_name S.Harder J.Spielmann data_hasj215 _database_code_depnum_ccdc_archive 'CCDC 822039' #TrackingRef '- hasj215c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common META-(Mg3(iPrN-BH-N(iPr)-BH3)2 _chemical_melting_point ? _chemical_formula_moiety 'C52 H88 B4 Mg3 N8, (C3 H7)' _chemical_formula_sum 'C55 H95 B4 Mg3 N8' _chemical_formula_weight 984.59 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' Mg Mg 0.0486 0.0363 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9417(12) _cell_length_b 16.6877(18) _cell_length_c 17.8037(19) _cell_angle_alpha 93.865(7) _cell_angle_beta 106.518(7) _cell_angle_gamma 103.888(7) _cell_volume 2993.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.142 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 0.094 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9569 _exptl_absorpt_correction_T_max 0.9738 _exptl_absorpt_process_details ; BRUKER AXS SMART APEX 2 Vers. 1.0-27 R.H. Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(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 ? _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 49723 _diffrn_reflns_av_R_equivalents 0.1233 _diffrn_reflns_av_sigmaI/netI 0.1174 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 26.15 _reflns_number_total 11850 _reflns_number_gt 6583 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.1150P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11850 _refine_ls_number_parameters 656 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1318 _refine_ls_R_factor_gt 0.0778 _refine_ls_wR_factor_ref 0.2166 _refine_ls_wR_factor_gt 0.1899 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _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 Mg1 Mg 0.18946(10) 0.70763(6) 0.50283(6) 0.0304(3) Uani 1 1 d . . . Mg2 Mg 0.15239(10) 0.73398(6) 0.17452(6) 0.0308(3) Uani 1 1 d . . . Mg3 Mg 0.08451(10) 0.78406(6) 0.33656(6) 0.0287(3) Uani 1 1 d . . . N1 N 0.2364(3) 0.67839(16) 0.61531(16) 0.0322(6) Uani 1 1 d . . . N2 N 0.2411(3) 0.60787(16) 0.46245(15) 0.0324(6) Uani 1 1 d . . . N3 N 0.2262(3) 0.63417(16) 0.18915(15) 0.0324(6) Uani 1 1 d . . . N4 N 0.1653(2) 0.73321(16) 0.06153(15) 0.0303(6) Uani 1 1 d . . . N5 N 0.2029(2) 0.82154(15) 0.46177(15) 0.0288(6) Uani 1 1 d . . . N6 N -0.0356(2) 0.79413(15) 0.41633(15) 0.0294(6) Uani 1 1 d . . . N7 N -0.0098(2) 0.74593(16) 0.20821(15) 0.0299(6) Uani 1 1 d . . . N8 N 0.1185(3) 0.88912(15) 0.26419(15) 0.0307(6) Uani 1 1 d . . . B1 B 0.0890(4) 0.8511(2) 0.4609(2) 0.0310(8) Uani 1 1 d . . . B2 B -0.0485(4) 0.6994(2) 0.4165(2) 0.0317(8) Uani 1 1 d . . . B3 B -0.0040(4) 0.8329(2) 0.2133(2) 0.0314(8) Uani 1 1 d . . . B4 B 0.2497(4) 0.8648(2) 0.2722(2) 0.0297(8) Uani 1 1 d . . . C1 C 0.1860(4) 0.5697(2) 0.6996(2) 0.0493(10) Uani 1 1 d . . . H1A H 0.2162 0.6177 0.7396 0.074 Uiso 1 1 calc R . . H1B H 0.2395 0.5321 0.7149 0.074 Uiso 1 1 calc R . . H1C H 0.0953 0.5421 0.6935 0.074 Uiso 1 1 calc R . . C2 C 0.1971(3) 0.5973(2) 0.6211(2) 0.0358(8) Uani 1 1 d . . . C3 C 0.1666(3) 0.5328(2) 0.5589(2) 0.0359(8) Uani 1 1 d . . . H3A H 0.1157 0.4813 0.5639 0.043 Uiso 1 1 calc R . . C4 C 0.2038(3) 0.5365(2) 0.4898(2) 0.0358(8) Uani 1 1 d . . . C5 C 0.2034(4) 0.4550(2) 0.4463(2) 0.0498(10) Uani 1 1 d . . . H5A H 0.1424 0.4096 0.4579 0.075 Uiso 1 1 calc R . . H5B H 0.2907 0.4471 0.4630 0.075 Uiso 1 1 calc R . . H5C H 0.1770 0.4567 0.3903 0.075 Uiso 1 1 calc R . . C6 C 0.3160(3) 0.7341(2) 0.68664(19) 0.0329(8) Uani 1 1 d . . . C7 C 0.4505(3) 0.7358(2) 0.7161(2) 0.0389(8) Uani 1 1 d . . . C8 C 0.5285(4) 0.7887(2) 0.7855(2) 0.0498(10) Uani 1 1 d . . . H8 H 0.6172 0.7898 0.8064 0.060 Uiso 1 1 calc R . . C9 C 0.4754(4) 0.8396(3) 0.8239(2) 0.0549(10) Uani 1 1 d . . . H9 H 0.5280 0.8734 0.8713 0.066 Uiso 1 1 calc R . . C10 C 0.3457(4) 0.8408(3) 0.7928(2) 0.0523(10) Uani 1 1 d . . . H10 H 0.3125 0.8766 0.8187 0.063 Uiso 1 1 calc R . . C11 C 0.2635(3) 0.7897(2) 0.7235(2) 0.0400(8) Uani 1 1 d . . . C12 C 0.5117(4) 0.6821(2) 0.6725(2) 0.0447(9) Uani 1 1 d . . . H12 H 0.4472 0.6588 0.6203 0.058 Uiso 1 1 calc R . . C13 C 0.5418(5) 0.6093(3) 0.7145(3) 0.0700(13) Uani 1 1 d . . . H13A H 0.5812 0.5783 0.6853 0.105 Uiso 1 1 calc R . . H13B H 0.4612 0.5735 0.7179 0.105 Uiso 1 1 calc R . . H13C H 0.6021 0.6302 0.7669 0.105 Uiso 1 1 calc R . . C14 C 0.6370(4) 0.7341(3) 0.6595(2) 0.0565(11) Uani 1 1 d . . . H14A H 0.6183 0.7807 0.6341 0.085 Uiso 1 1 calc R . . H14B H 0.6669 0.7003 0.6265 0.085 Uiso 1 1 calc R . . H14C H 0.7046 0.7540 0.7096 0.085 Uiso 1 1 calc R . . C15 C 0.1234(4) 0.7946(3) 0.6879(2) 0.0612(12) Uani 1 1 d . . . H15 H 0.0945 0.7718 0.6316 0.079 Uiso 1 1 calc R . . C16 C 0.1095(5) 0.8834(3) 0.6940(3) 0.0874(17) Uani 1 1 d . . . H16A H 0.1202 0.9032 0.7480 0.131 Uiso 1 1 calc R . . H16B H 0.0234 0.8838 0.6610 0.131 Uiso 1 1 calc R . . H16C H 0.1762 0.9189 0.6768 0.131 Uiso 1 1 calc R . . C17 C 0.0310(5) 0.7427(4) 0.7255(5) 0.126(3) Uani 1 1 d . . . H17A H 0.0424 0.6874 0.7249 0.189 Uiso 1 1 calc R . . H17B H -0.0588 0.7399 0.6964 0.189 Uiso 1 1 calc R . . H17C H 0.0504 0.7676 0.7792 0.189 Uiso 1 1 calc R . . C18 C 0.3049(3) 0.60913(19) 0.40250(19) 0.0319(7) Uani 1 1 d . . . C19 C 0.4367(3) 0.6111(2) 0.4210(2) 0.0382(8) Uani 1 1 d . . . H19 H 0.4839 0.6073 0.4725 0.046 Uiso 1 1 calc R . . C20 C 0.4996(3) 0.6185(2) 0.3630(2) 0.0438(9) Uani 1 1 d . . . H20 H 0.5884 0.6193 0.3759 0.053 Uiso 1 1 calc R . . C21 C 0.4303(3) 0.6247(2) 0.2861(2) 0.0381(8) Uani 1 1 d . . . H21 H 0.4731 0.6305 0.2478 0.046 Uiso 1 1 calc R . . C22 C 0.2975(3) 0.62222(19) 0.26657(19) 0.0333(7) Uani 1 1 d . . . C23 C 0.2351(3) 0.61461(19) 0.32524(19) 0.0322(7) Uani 1 1 d . . . H23 H 0.1460 0.6132 0.3125 0.042 Uiso 1 1 calc R . . C24 C 0.2027(4) 0.4875(2) 0.1438(2) 0.0557(11) Uani 1 1 d . . . H24A H 0.2914 0.4889 0.1738 0.083 Uiso 1 1 calc R . . H24B H 0.1769 0.4514 0.0944 0.083 Uiso 1 1 calc R . . H24C H 0.1435 0.4670 0.1732 0.083 Uiso 1 1 calc R . . C25 C 0.1968(3) 0.5747(2) 0.1278(2) 0.0375(8) Uani 1 1 d . . . C26 C 0.1588(3) 0.5879(2) 0.0494(2) 0.0395(8) Uani 1 1 d . . . H26 H 0.1269 0.5401 0.0120 0.047 Uiso 1 1 calc R . . C27 C 0.1618(3) 0.6637(2) 0.01861(19) 0.0334(7) Uani 1 1 d . . . C28 C 0.1668(4) 0.6634(2) -0.0650(2) 0.0461(9) Uani 1 1 d . . . H28A H 0.1537 0.7146 -0.0829 0.069 Uiso 1 1 calc R . . H28B H 0.0983 0.6172 -0.0987 0.069 Uiso 1 1 calc R . . H28C H 0.2515 0.6582 -0.0667 0.069 Uiso 1 1 calc R . . C29 C 0.1884(3) 0.8112(2) 0.03097(18) 0.0306(7) Uani 1 1 d . . . C30 C 0.0795(3) 0.8387(2) -0.0107(2) 0.0406(8) Uani 1 1 d . . . C31 C 0.1055(4) 0.9149(2) -0.0398(2) 0.0512(10) Uani 1 1 d . . . H31 H 0.0354 0.9335 -0.0690 0.061 Uiso 1 1 calc R . . C32 C 0.2328(4) 0.9622(2) -0.0256(2) 0.0566(11) Uani 1 1 d . . . H32 H 0.2486 1.0119 -0.0464 0.068 Uiso 1 1 calc R . . C33 C 0.3369(4) 0.9369(2) 0.0189(2) 0.0537(10) Uani 1 1 d . . . H33 H 0.4225 0.9710 0.0298 0.064 Uiso 1 1 calc R . . C34 C 0.3177(3) 0.8607(2) 0.0485(2) 0.0405(8) Uani 1 1 d . . . C35 C -0.0622(4) 0.7880(3) -0.0255(2) 0.0509(10) Uani 1 1 d . . . H35 H -0.0607 0.7452 0.0095 0.066 Uiso 1 1 calc R . . C36 C -0.1266(4) 0.7440(3) -0.1103(3) 0.0703(13) Uani 1 1 d . . . H36A H -0.1283 0.7847 -0.1459 0.105 Uiso 1 1 calc R . . H36B H -0.2155 0.7122 -0.1167 0.105 Uiso 1 1 calc R . . H36C H -0.0767 0.7073 -0.1217 0.105 Uiso 1 1 calc R . . C37 C -0.1492(4) 0.8412(3) -0.0065(2) 0.0625(12) Uani 1 1 d . . . H37A H -0.1080 0.8710 0.0463 0.094 Uiso 1 1 calc R . . H37B H -0.2346 0.8056 -0.0103 0.094 Uiso 1 1 calc R . . H37C H -0.1595 0.8802 -0.0435 0.094 Uiso 1 1 calc R . . C38 C 0.4378(3) 0.8360(3) 0.0974(2) 0.0523(10) Uani 1 1 d . . . H38 H 0.4058 0.7866 0.1205 0.068 Uiso 1 1 calc R . . C39 C 0.5298(4) 0.9044(3) 0.1656(3) 0.0742(14) Uani 1 1 d . . . H39A H 0.5642 0.9531 0.1444 0.111 Uiso 1 1 calc R . . H39B H 0.6017 0.8847 0.1956 0.111 Uiso 1 1 calc R . . H39C H 0.4810 0.9180 0.1994 0.111 Uiso 1 1 calc R . . C40 C 0.5170(4) 0.8126(3) 0.0449(3) 0.0712(13) Uani 1 1 d . . . H40A H 0.4595 0.7700 0.0021 0.107 Uiso 1 1 calc R . . H40B H 0.5873 0.7921 0.0758 0.107 Uiso 1 1 calc R . . H40C H 0.5537 0.8609 0.0240 0.107 Uiso 1 1 calc R . . C41 C 0.3375(3) 0.8810(2) 0.49034(19) 0.0317(7) Uani 1 1 d . . . H41 H 0.3401 0.9236 0.4551 0.041 Uiso 1 1 calc R . . C42 C 0.4398(3) 0.8355(2) 0.4845(2) 0.0432(9) Uani 1 1 d . . . H42A H 0.4411 0.7944 0.5197 0.065 Uiso 1 1 calc R . . H42B H 0.5256 0.8748 0.4990 0.065 Uiso 1 1 calc R . . H42C H 0.4175 0.8086 0.4312 0.065 Uiso 1 1 calc R . . C43 C 0.3718(4) 0.9249(2) 0.5738(2) 0.0464(9) Uani 1 1 d . . . H43A H 0.3075 0.9544 0.5763 0.070 Uiso 1 1 calc R . . H43B H 0.4581 0.9637 0.5883 0.070 Uiso 1 1 calc R . . H43C H 0.3717 0.8845 0.6097 0.070 Uiso 1 1 calc R . . C44 C -0.1617(3) 0.8169(2) 0.4081(2) 0.0384(8) Uani 1 1 d . . . H44 H -0.2321 0.7739 0.3687 0.050 Uiso 1 1 calc R . . C45 C -0.1952(4) 0.8151(3) 0.4852(2) 0.0598(11) Uani 1 1 d . . . H45A H -0.1949 0.7619 0.5026 0.090 Uiso 1 1 calc R . . H45B H -0.2814 0.8238 0.4770 0.090 Uiso 1 1 calc R . . H45C H -0.1306 0.8584 0.5247 0.090 Uiso 1 1 calc R . . C46 C -0.1607(4) 0.9002(2) 0.3772(2) 0.0525(10) Uani 1 1 d . . . H46A H -0.0965 0.9445 0.4159 0.079 Uiso 1 1 calc R . . H46B H -0.2468 0.9094 0.3673 0.079 Uiso 1 1 calc R . . H46C H -0.1381 0.8990 0.3289 0.079 Uiso 1 1 calc R . . C47 C -0.1402(3) 0.6877(2) 0.1635(2) 0.0383(8) Uani 1 1 d . . . H47 H -0.1754 0.7101 0.1148 0.050 Uiso 1 1 calc R . . C48 C -0.1255(4) 0.6021(2) 0.1394(3) 0.0603(12) Uani 1 1 d . . . H48A H -0.0735 0.6066 0.1039 0.090 Uiso 1 1 calc R . . H48B H -0.2115 0.5645 0.1136 0.090 Uiso 1 1 calc R . . H48C H -0.0823 0.5812 0.1858 0.090 Uiso 1 1 calc R . . C49 C -0.2405(4) 0.6792(3) 0.2084(2) 0.0556(11) Uani 1 1 d . . . H49A H -0.2083 0.6577 0.2567 0.083 Uiso 1 1 calc R . . H49B H -0.3231 0.6417 0.1764 0.083 Uiso 1 1 calc R . . H49C H -0.2533 0.7329 0.2206 0.083 Uiso 1 1 calc R . . C50 C 0.1272(3) 0.97975(19) 0.2682(2) 0.0375(8) Uani 1 1 d . . . H50 H 0.0366 0.9852 0.2557 0.049 Uiso 1 1 calc R . . C51 C 0.1850(4) 1.0171(2) 0.2053(2) 0.0543(10) Uani 1 1 d . . . H51A H 0.2765 1.0176 0.2186 0.082 Uiso 1 1 calc R . . H51B H 0.1775 1.0732 0.2035 0.082 Uiso 1 1 calc R . . H51C H 0.1370 0.9840 0.1545 0.082 Uiso 1 1 calc R . . C52 C 0.2041(4) 1.0286(2) 0.3498(2) 0.0447(9) Uani 1 1 d . . . H52A H 0.1670 1.0038 0.3883 0.067 Uiso 1 1 calc R . . H52B H 0.1989 1.0852 0.3503 0.067 Uiso 1 1 calc R . . H52C H 0.2951 1.0277 0.3624 0.067 Uiso 1 1 calc R . . H106 H 0.349(3) 0.9121(17) 0.3128(16) 0.028(7) Uiso 1 1 d . . . H105 H 0.238(3) 0.7997(18) 0.2990(16) 0.023(7) Uiso 1 1 d . . . H107 H 0.256(3) 0.8479(17) 0.2112(16) 0.029(7) Uiso 1 1 d . . . H103 H -0.146(3) 0.6636(18) 0.3936(16) 0.021(7) Uiso 1 1 d . . . H104 H -0.090(3) 0.854(2) 0.185(2) 0.048(10) Uiso 1 1 d . . . H100 H 0.098(3) 0.919(2) 0.4881(18) 0.038(9) Uiso 1 1 d . . . H101 H 0.011(3) 0.6812(19) 0.3769(18) 0.036(8) Uiso 1 1 d . . . H102 H -0.008(4) 0.680(2) 0.483(2) 0.064(11) 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 Mg1 0.0340(6) 0.0270(6) 0.0349(6) 0.0112(5) 0.0108(5) 0.0149(5) Mg2 0.0364(6) 0.0269(6) 0.0350(6) 0.0088(5) 0.0126(5) 0.0165(5) Mg3 0.0314(6) 0.0247(5) 0.0336(6) 0.0079(5) 0.0107(5) 0.0127(4) N1 0.0345(15) 0.0276(14) 0.0382(16) 0.0115(13) 0.0108(13) 0.0140(12) N2 0.0399(15) 0.0251(14) 0.0377(16) 0.0124(12) 0.0123(13) 0.0164(12) N3 0.0398(15) 0.0290(15) 0.0345(16) 0.0117(13) 0.0127(13) 0.0174(12) N4 0.0355(15) 0.0252(14) 0.0322(15) 0.0054(12) 0.0092(12) 0.0128(12) N5 0.0291(14) 0.0244(13) 0.0358(15) 0.0079(12) 0.0100(12) 0.0116(11) N6 0.0289(14) 0.0273(14) 0.0378(15) 0.0094(12) 0.0106(12) 0.0165(12) N7 0.0322(14) 0.0248(14) 0.0352(15) 0.0040(12) 0.0110(12) 0.0115(11) N8 0.0379(15) 0.0209(13) 0.0363(15) 0.0070(12) 0.0097(12) 0.0150(12) B1 0.036(2) 0.030(2) 0.034(2) 0.0111(17) 0.0124(17) 0.0168(17) B2 0.0251(19) 0.030(2) 0.042(2) 0.0093(18) 0.0093(17) 0.0103(16) B3 0.036(2) 0.030(2) 0.036(2) 0.0097(17) 0.0150(18) 0.0186(17) B4 0.032(2) 0.0265(19) 0.032(2) 0.0036(17) 0.0082(17) 0.0122(16) C1 0.063(2) 0.040(2) 0.051(2) 0.0195(19) 0.024(2) 0.0139(19) C2 0.0337(18) 0.0372(19) 0.042(2) 0.0217(17) 0.0137(16) 0.0143(15) C3 0.0369(18) 0.0277(17) 0.044(2) 0.0134(16) 0.0136(16) 0.0058(15) C4 0.0310(17) 0.0270(17) 0.048(2) 0.0125(16) 0.0070(16) 0.0102(14) C5 0.068(3) 0.0258(18) 0.062(3) 0.0130(18) 0.027(2) 0.0149(18) C6 0.0393(19) 0.0332(18) 0.0307(18) 0.0128(15) 0.0108(15) 0.0158(15) C7 0.045(2) 0.0313(18) 0.045(2) 0.0085(17) 0.0132(17) 0.0186(16) C8 0.042(2) 0.049(2) 0.056(3) 0.001(2) 0.0054(19) 0.0211(18) C9 0.058(3) 0.053(3) 0.043(2) -0.005(2) 0.001(2) 0.018(2) C10 0.070(3) 0.051(2) 0.044(2) 0.006(2) 0.018(2) 0.033(2) C11 0.047(2) 0.045(2) 0.035(2) 0.0108(17) 0.0122(17) 0.0237(17) C12 0.041(2) 0.040(2) 0.050(2) -0.0033(18) 0.0035(17) 0.0207(17) C13 0.075(3) 0.043(2) 0.102(4) 0.017(2) 0.027(3) 0.034(2) C14 0.049(2) 0.065(3) 0.059(3) 0.009(2) 0.013(2) 0.027(2) C15 0.061(3) 0.088(3) 0.038(2) -0.008(2) 0.008(2) 0.042(3) C16 0.085(4) 0.104(4) 0.110(4) 0.051(3) 0.041(3) 0.071(3) C17 0.058(3) 0.099(5) 0.244(8) 0.066(5) 0.055(4) 0.042(3) C18 0.0358(18) 0.0218(16) 0.0394(19) 0.0066(14) 0.0093(15) 0.0123(14) C19 0.0392(19) 0.038(2) 0.039(2) 0.0112(16) 0.0083(16) 0.0178(16) C20 0.0321(18) 0.048(2) 0.059(2) 0.0133(19) 0.0150(17) 0.0207(17) C21 0.042(2) 0.038(2) 0.045(2) 0.0133(17) 0.0197(17) 0.0201(16) C22 0.0383(18) 0.0223(16) 0.042(2) 0.0100(15) 0.0120(16) 0.0130(14) C23 0.0318(17) 0.0251(17) 0.045(2) 0.0116(15) 0.0115(15) 0.0153(14) C24 0.073(3) 0.031(2) 0.061(3) 0.0098(19) 0.010(2) 0.022(2) C25 0.0383(19) 0.0306(18) 0.044(2) 0.0063(17) 0.0095(16) 0.0145(15) C26 0.045(2) 0.0267(18) 0.045(2) -0.0005(16) 0.0072(17) 0.0171(16) C27 0.0301(17) 0.0346(19) 0.0331(18) -0.0017(15) 0.0021(14) 0.0151(15) C28 0.059(2) 0.049(2) 0.038(2) 0.0052(18) 0.0117(18) 0.0329(19) C29 0.0431(19) 0.0289(17) 0.0263(17) 0.0069(14) 0.0132(15) 0.0181(15) C30 0.047(2) 0.040(2) 0.040(2) 0.0134(17) 0.0120(17) 0.0211(17) C31 0.062(3) 0.043(2) 0.060(3) 0.026(2) 0.020(2) 0.029(2) C32 0.075(3) 0.037(2) 0.071(3) 0.028(2) 0.033(2) 0.022(2) C33 0.054(2) 0.044(2) 0.064(3) 0.012(2) 0.026(2) 0.0042(19) C34 0.042(2) 0.040(2) 0.047(2) 0.0138(17) 0.0212(17) 0.0150(17) C35 0.043(2) 0.054(2) 0.063(3) 0.030(2) 0.0098(19) 0.0283(19) C36 0.056(3) 0.045(2) 0.104(4) -0.005(3) 0.015(3) 0.021(2) C37 0.051(2) 0.088(3) 0.054(3) 0.012(2) 0.015(2) 0.032(2) C38 0.033(2) 0.066(3) 0.059(3) 0.023(2) 0.0150(19) 0.0114(19) C39 0.043(2) 0.111(4) 0.061(3) 0.004(3) 0.011(2) 0.015(3) C40 0.056(3) 0.072(3) 0.088(4) 0.004(3) 0.020(2) 0.029(2) C41 0.0282(16) 0.0305(17) 0.0385(19) 0.0132(15) 0.0082(14) 0.0123(14) C42 0.0301(18) 0.040(2) 0.056(2) 0.0034(18) 0.0058(17) 0.0135(16) C43 0.038(2) 0.046(2) 0.052(2) -0.0037(19) 0.0130(18) 0.0091(17) C44 0.0332(18) 0.039(2) 0.045(2) 0.0040(17) 0.0084(16) 0.0190(16) C45 0.047(2) 0.084(3) 0.058(3) 0.005(2) 0.020(2) 0.033(2) C46 0.049(2) 0.042(2) 0.071(3) 0.008(2) 0.009(2) 0.0317(18) C47 0.0335(18) 0.0352(19) 0.043(2) 0.0023(16) 0.0074(16) 0.0103(15) C48 0.044(2) 0.036(2) 0.093(3) -0.011(2) 0.018(2) 0.0057(18) C49 0.037(2) 0.067(3) 0.059(3) -0.001(2) 0.0177(19) 0.0056(19) C50 0.044(2) 0.0234(17) 0.048(2) 0.0110(16) 0.0098(17) 0.0179(15) C51 0.079(3) 0.033(2) 0.053(2) 0.0205(19) 0.016(2) 0.021(2) C52 0.053(2) 0.0261(18) 0.056(2) 0.0041(17) 0.0134(19) 0.0173(17) _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 Mg1 N2 2.032(3) . ? Mg1 N1 2.044(3) . ? Mg1 N5 2.070(3) . ? Mg1 B2 2.586(4) . ? Mg1 Mg3 3.3148(14) . ? Mg1 H102 2.01(4) . ? Mg2 N3 2.020(3) . ? Mg2 N4 2.056(3) . ? Mg2 N7 2.076(3) . ? Mg2 B4 2.498(4) . ? Mg2 B3 2.830(4) . ? Mg2 Mg3 3.2807(15) . ? Mg2 H105 2.23(3) . ? Mg2 H107 1.92(3) . ? Mg3 N5 2.196(3) . ? Mg3 N7 2.200(3) . ? Mg3 N6 2.215(3) . ? Mg3 N8 2.266(3) . ? Mg3 B1 2.395(4) . ? Mg3 B3 2.414(4) . ? Mg3 B2 2.569(4) . ? Mg3 B4 2.572(4) . ? Mg3 H105 1.94(3) . ? Mg3 H101 1.98(3) . ? N1 C2 1.339(4) . ? N1 C6 1.434(4) . ? N2 C4 1.334(4) . ? N2 C18 1.430(4) . ? N3 C25 1.336(4) . ? N3 C22 1.431(4) . ? N4 C27 1.332(4) . ? N4 C29 1.439(4) . ? N5 B1 1.443(4) . ? N5 C41 1.488(4) . ? N6 B1 1.433(5) . ? N6 C44 1.488(4) . ? N6 B2 1.552(4) . ? N7 B3 1.433(4) . ? N7 C47 1.483(4) . ? N8 B3 1.445(5) . ? N8 C50 1.488(4) . ? N8 B4 1.555(4) . ? B1 H100 1.17(3) . ? B2 H103 1.04(3) . ? B2 H101 1.16(3) . ? B2 H102 1.23(4) . ? B3 H104 1.09(4) . ? B4 H106 1.18(3) . ? B4 H105 1.21(3) . ? B4 H107 1.13(3) . ? C1 C2 1.528(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.397(5) . ? C3 C4 1.401(5) . ? C3 H3A 0.9300 . ? C4 C5 1.519(5) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.407(5) . ? C6 C11 1.418(5) . ? C7 C8 1.388(5) . ? C7 C12 1.532(5) . ? C8 C9 1.383(5) . ? C8 H8 0.9300 . ? C9 C10 1.374(6) . ? C9 H9 0.9300 . ? C10 C11 1.385(5) . ? C10 H10 0.9300 . ? C11 C15 1.507(5) . ? C12 C13 1.523(5) . ? C12 C14 1.523(5) . ? C12 H12 0.9800 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C17 1.505(7) . ? C15 C16 1.525(6) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.377(4) . ? C18 C23 1.391(4) . ? C19 C20 1.390(5) . ? C19 H19 0.9300 . ? C20 C21 1.388(5) . ? C20 H20 0.9300 . ? C21 C22 1.384(5) . ? C21 H21 0.9300 . ? C22 C23 1.398(4) . ? C23 H23 0.9300 . ? C24 C25 1.513(5) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.387(5) . ? C26 C27 1.408(5) . ? C26 H26 0.9300 . ? C27 C28 1.504(5) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C34 1.390(5) . ? C29 C30 1.410(5) . ? C30 C31 1.400(5) . ? C30 C35 1.515(5) . ? C31 C32 1.369(5) . ? C31 H31 0.9300 . ? C32 C33 1.366(6) . ? C32 H32 0.9300 . ? C33 C34 1.402(5) . ? C33 H33 0.9300 . ? C34 C38 1.521(5) . ? C35 C36 1.521(6) . ? C35 C37 1.535(5) . ? C35 H35 0.9800 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 C40 1.533(6) . ? C38 C39 1.534(6) . ? C38 H38 0.9800 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C43 1.513(5) . ? C41 C42 1.518(4) . ? C41 H41 0.9800 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 C45 1.518(5) . ? C44 C46 1.529(5) . ? C44 H44 0.9800 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 C49 1.518(5) . ? C47 C48 1.523(5) . ? C47 H47 0.9800 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 C52 1.516(5) . ? C50 C51 1.533(5) . ? C50 H50 0.9800 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Mg1 N1 91.12(11) . . ? N2 Mg1 N5 128.15(11) . . ? N1 Mg1 N5 131.26(12) . . ? N2 Mg1 B2 108.01(12) . . ? N1 Mg1 B2 124.08(12) . . ? N5 Mg1 B2 74.98(11) . . ? N2 Mg1 Mg3 101.17(8) . . ? N1 Mg1 Mg3 167.49(9) . . ? N5 Mg1 Mg3 40.39(8) . . ? B2 Mg1 Mg3 49.76(8) . . ? N2 Mg1 H102 110.5(11) . . ? N1 Mg1 H102 96.4(11) . . ? N5 Mg1 H102 94.8(11) . . ? B2 Mg1 H102 27.7(11) . . ? Mg3 Mg1 H102 77.2(11) . . ? N3 Mg2 N4 91.42(11) . . ? N3 Mg2 N7 123.28(11) . . ? N4 Mg2 N7 125.60(11) . . ? N3 Mg2 B4 121.57(12) . . ? N4 Mg2 B4 120.53(12) . . ? N7 Mg2 B4 78.31(11) . . ? N3 Mg2 B3 149.82(11) . . ? N4 Mg2 B3 115.41(11) . . ? N7 Mg2 B3 29.13(10) . . ? B4 Mg2 B3 57.50(12) . . ? N3 Mg2 Mg3 107.55(8) . . ? N4 Mg2 Mg3 160.94(8) . . ? N7 Mg2 Mg3 41.30(8) . . ? B4 Mg2 Mg3 50.66(9) . . ? B3 Mg2 Mg3 45.81(8) . . ? N3 Mg2 H105 98.7(8) . . ? N4 Mg2 H105 145.4(7) . . ? N7 Mg2 H105 75.0(7) . . ? B4 Mg2 H105 28.9(7) . . ? B3 Mg2 H105 67.5(7) . . ? Mg3 Mg2 H105 35.2(7) . . ? N3 Mg2 H107 124.2(8) . . ? N4 Mg2 H107 95.2(8) . . ? N7 Mg2 H107 96.3(8) . . ? B4 Mg2 H107 25.6(8) . . ? B3 Mg2 H107 69.5(8) . . ? Mg3 Mg2 H107 75.9(8) . . ? H105 Mg2 H107 52.0(10) . . ? N5 Mg3 N7 172.52(10) . . ? N5 Mg3 N6 66.51(9) . . ? N7 Mg3 N6 120.94(10) . . ? N5 Mg3 N8 112.01(10) . . ? N7 Mg3 N8 66.17(9) . . ? N6 Mg3 N8 116.89(10) . . ? N5 Mg3 B1 36.31(11) . . ? N7 Mg3 B1 150.59(12) . . ? N6 Mg3 B1 35.95(11) . . ? N8 Mg3 B1 104.68(11) . . ? N5 Mg3 B3 145.19(12) . . ? N7 Mg3 B3 35.81(11) . . ? N6 Mg3 B3 110.71(11) . . ? N8 Mg3 B3 35.80(11) . . ? B1 Mg3 B3 121.96(13) . . ? N5 Mg3 B2 73.40(11) . . ? N7 Mg3 B2 111.90(12) . . ? N6 Mg3 B2 36.94(10) . . ? N8 Mg3 B2 150.88(11) . . ? B1 Mg3 B2 61.79(13) . . ? B3 Mg3 B2 126.73(13) . . ? N5 Mg3 B4 99.57(11) . . ? N7 Mg3 B4 74.60(11) . . ? N6 Mg3 B4 145.57(11) . . ? N8 Mg3 B4 36.81(10) . . ? B1 Mg3 B4 115.80(13) . . ? B3 Mg3 B4 62.20(12) . . ? B2 Mg3 B4 171.00(13) . . ? N5 Mg3 Mg2 134.01(8) . . ? N7 Mg3 Mg2 38.51(7) . . ? N6 Mg3 Mg2 158.72(8) . . ? N8 Mg3 Mg2 65.06(7) . . ? B1 Mg3 Mg2 164.23(10) . . ? B3 Mg3 Mg2 57.18(9) . . ? B2 Mg3 Mg2 132.88(10) . . ? B4 Mg3 Mg2 48.71(9) . . ? N5 Mg3 Mg1 37.65(7) . . ? N7 Mg3 Mg1 141.84(8) . . ? N6 Mg3 Mg1 67.90(7) . . ? N8 Mg3 Mg1 147.64(8) . . ? B1 Mg3 Mg1 58.94(9) . . ? B3 Mg3 Mg1 176.54(10) . . ? B2 Mg3 Mg1 50.21(9) . . ? B4 Mg3 Mg1 120.83(9) . . ? Mg2 Mg3 Mg1 123.03(4) . . ? N5 Mg3 H105 94.2(8) . . ? N7 Mg3 H105 78.4(8) . . ? N6 Mg3 H105 159.7(8) . . ? N8 Mg3 H105 63.0(9) . . ? B1 Mg3 H105 123.9(8) . . ? B3 Mg3 H105 81.1(8) . . ? B2 Mg3 H105 146.1(9) . . ? B4 Mg3 H105 26.7(9) . . ? Mg2 Mg3 H105 41.5(8) . . ? Mg1 Mg3 H105 101.2(8) . . ? N5 Mg3 H101 81.9(9) . . ? N7 Mg3 H101 100.7(9) . . ? N6 Mg3 H101 62.6(9) . . ? N8 Mg3 H101 165.1(9) . . ? B1 Mg3 H101 83.2(9) . . ? B3 Mg3 H101 129.3(9) . . ? B2 Mg3 H101 25.7(9) . . ? B4 Mg3 H101 149.7(9) . . ? Mg2 Mg3 H101 109.6(9) . . ? Mg1 Mg3 H101 47.2(9) . . ? H105 Mg3 H101 123.2(13) . . ? C2 N1 C6 117.4(3) . . ? C2 N1 Mg1 115.5(2) . . ? C6 N1 Mg1 126.87(19) . . ? C4 N2 C18 119.4(3) . . ? C4 N2 Mg1 117.1(2) . . ? C18 N2 Mg1 123.34(19) . . ? C25 N3 C22 119.5(3) . . ? C25 N3 Mg2 119.9(2) . . ? C22 N3 Mg2 120.2(2) . . ? C27 N4 C29 119.7(3) . . ? C27 N4 Mg2 121.6(2) . . ? C29 N4 Mg2 118.52(19) . . ? B1 N5 C41 119.6(3) . . ? B1 N5 Mg1 111.28(19) . . ? C41 N5 Mg1 114.78(18) . . ? B1 N5 Mg3 79.39(19) . . ? C41 N5 Mg3 124.29(18) . . ? Mg1 N5 Mg3 101.96(11) . . ? B1 N6 C44 120.7(3) . . ? B1 N6 B2 117.5(3) . . ? C44 N6 B2 113.9(2) . . ? B1 N6 Mg3 78.86(18) . . ? C44 N6 Mg3 134.6(2) . . ? B2 N6 Mg3 84.01(17) . . ? B3 N7 C47 115.8(3) . . ? B3 N7 Mg2 106.04(19) . . ? C47 N7 Mg2 117.20(19) . . ? B3 N7 Mg3 80.29(19) . . ? C47 N7 Mg3 130.3(2) . . ? Mg2 N7 Mg3 100.19(11) . . ? B3 N8 C50 116.3(3) . . ? B3 N8 B4 118.5(3) . . ? C50 N8 B4 116.3(3) . . ? B3 N8 Mg3 77.69(18) . . ? C50 N8 Mg3 139.6(2) . . ? B4 N8 Mg3 82.34(17) . . ? N6 B1 N5 114.5(3) . . ? N6 B1 Mg3 65.19(17) . . ? N5 B1 Mg3 64.30(17) . . ? N6 B1 H100 122.4(16) . . ? N5 B1 H100 122.7(16) . . ? Mg3 B1 H100 136.3(15) . . ? N6 B2 Mg3 59.05(15) . . ? N6 B2 Mg1 99.1(2) . . ? Mg3 B2 Mg1 80.03(11) . . ? N6 B2 H103 112.3(16) . . ? Mg3 B2 H103 124.9(15) . . ? Mg1 B2 H103 146.8(16) . . ? N6 B2 H101 106.8(16) . . ? Mg3 B2 H101 47.7(15) . . ? Mg1 B2 H101 70.1(15) . . ? H103 B2 H101 109(2) . . ? N6 B2 H102 114.3(19) . . ? Mg3 B2 H102 128.6(17) . . ? Mg1 B2 H102 49.3(17) . . ? H103 B2 H102 105(2) . . ? H101 B2 H102 109(2) . . ? N7 B3 N8 115.8(3) . . ? N7 B3 Mg3 63.90(17) . . ? N8 B3 Mg3 66.51(17) . . ? N7 B3 Mg2 44.83(14) . . ? N8 B3 Mg2 86.73(19) . . ? Mg3 B3 Mg2 77.01(11) . . ? N7 B3 H104 121.7(19) . . ? N8 B3 H104 122.2(19) . . ? Mg3 B3 H104 137.2(17) . . ? Mg2 B3 H104 140.0(18) . . ? N8 B4 Mg2 97.2(2) . . ? N8 B4 Mg3 60.85(15) . . ? Mg2 B4 Mg3 80.63(11) . . ? N8 B4 H106 117.4(13) . . ? Mg2 B4 H106 145.1(13) . . ? Mg3 B4 H106 119.1(12) . . ? N8 B4 H105 105.9(13) . . ? Mg2 B4 H105 63.3(13) . . ? Mg3 B4 H105 46.3(13) . . ? H106 B4 H105 108.0(18) . . ? N8 B4 H107 109.3(14) . . ? Mg2 B4 H107 47.5(13) . . ? Mg3 B4 H107 127.1(13) . . ? H106 B4 H107 111.2(18) . . ? H105 B4 H107 104.1(19) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 124.1(3) . . ? N1 C2 C1 120.4(3) . . ? C3 C2 C1 115.5(3) . . ? C2 C3 C4 127.6(3) . . ? C2 C3 H3A 116.2 . . ? C4 C3 H3A 116.2 . . ? N2 C4 C3 123.0(3) . . ? N2 C4 C5 119.6(3) . . ? C3 C4 C5 117.4(3) . . ? 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 C11 120.8(3) . . ? C7 C6 N1 117.9(3) . . ? C11 C6 N1 121.2(3) . . ? C8 C7 C6 118.6(3) . . ? C8 C7 C12 120.0(3) . . ? C6 C7 C12 121.4(3) . . ? C9 C8 C7 120.5(4) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C10 C9 C8 120.6(4) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 121.3(4) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C10 C11 C6 117.9(3) . . ? C10 C11 C15 120.7(3) . . ? C6 C11 C15 121.4(3) . . ? C13 C12 C14 109.6(3) . . ? C13 C12 C7 112.9(3) . . ? C14 C12 C7 111.5(3) . . ? C13 C12 H12 107.6 . . ? C14 C12 H12 107.6 . . ? C7 C12 H12 107.6 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 C11 111.4(4) . . ? C17 C15 C16 108.5(4) . . ? C11 C15 C16 113.5(4) . . ? C17 C15 H15 107.7 . . ? C11 C15 H15 107.7 . . ? C16 C15 H15 107.7 . . ? 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 C23 119.3(3) . . ? C19 C18 N2 121.1(3) . . ? C23 C18 N2 119.4(3) . . ? C18 C19 C20 120.3(3) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C21 C20 C19 120.3(3) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C22 C21 C20 120.0(3) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 119.2(3) . . ? C21 C22 N3 121.0(3) . . ? C23 C22 N3 119.5(3) . . ? C18 C23 C22 120.8(3) . . ? C18 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C25 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C25 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C25 C26 123.5(3) . . ? N3 C25 C24 118.8(3) . . ? C26 C25 C24 117.7(3) . . ? C25 C26 C27 129.1(3) . . ? C25 C26 H26 115.5 . . ? C27 C26 H26 115.5 . . ? N4 C27 C26 122.4(3) . . ? N4 C27 C28 121.1(3) . . ? C26 C27 C28 116.5(3) . . ? 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 . . ? C34 C29 C30 121.4(3) . . ? C34 C29 N4 119.0(3) . . ? C30 C29 N4 119.4(3) . . ? C31 C30 C29 117.9(3) . . ? C31 C30 C35 120.1(3) . . ? C29 C30 C35 122.0(3) . . ? C32 C31 C30 120.8(3) . . ? C32 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? C33 C32 C31 120.5(3) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C32 C33 C34 121.5(4) . . ? C32 C33 H33 119.3 . . ? C34 C33 H33 119.3 . . ? C29 C34 C33 117.7(3) . . ? C29 C34 C38 123.4(3) . . ? C33 C34 C38 118.9(3) . . ? C30 C35 C36 112.4(3) . . ? C30 C35 C37 112.4(3) . . ? C36 C35 C37 108.6(3) . . ? C30 C35 H35 107.8 . . ? C36 C35 H35 107.8 . . ? C37 C35 H35 107.8 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 C40 110.7(3) . . ? C34 C38 C39 113.1(4) . . ? C40 C38 C39 109.3(3) . . ? C34 C38 H38 107.8 . . ? C40 C38 H38 107.8 . . ? C39 C38 H38 107.8 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N5 C41 C43 113.2(2) . . ? N5 C41 C42 109.7(3) . . ? C43 C41 C42 110.4(3) . . ? N5 C41 H41 107.8 . . ? C43 C41 H41 107.8 . . ? C42 C41 H41 107.8 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N6 C44 C45 110.9(3) . . ? N6 C44 C46 112.3(3) . . ? C45 C44 C46 112.1(3) . . ? N6 C44 H44 107.1 . . ? C45 C44 H44 107.1 . . ? C46 C44 H44 107.1 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N7 C47 C49 113.1(3) . . ? N7 C47 C48 110.9(3) . . ? C49 C47 C48 109.9(3) . . ? N7 C47 H47 107.6 . . ? C49 C47 H47 107.6 . . ? C48 C47 H47 107.6 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N8 C50 C52 113.1(3) . . ? N8 C50 C51 110.7(3) . . ? C52 C50 C51 110.9(3) . . ? N8 C50 H50 107.3 . . ? C52 C50 H50 107.3 . . ? C51 C50 H50 107.3 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.500 0.000 194 36 ' ' 2 0.480 0.177 0.687 16 0 ' ' 3 0.520 0.823 0.313 16 0 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.15 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.601 _refine_diff_density_min -0.497 _refine_diff_density_rms 0.080 # Attachment '- hasj235c.cif' data_hasj235 _database_code_depnum_ccdc_archive 'CCDC 822040' #TrackingRef '- hasj235c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (META-Mg)2 _chemical_melting_point ? _chemical_formula_moiety 'C80 H104 Mg2 N8, 3(C6 H6)' _chemical_formula_sum 'C98 H122 Mg2 N8' _chemical_formula_weight 1460.71 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' N N 0.0061 0.0033 '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' _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 19.0122(13) _cell_length_b 22.8562(15) _cell_length_c 20.8328(14) _cell_angle_alpha 90.00 _cell_angle_beta 110.058(2) _cell_angle_gamma 90.00 _cell_volume 8503.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.141 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2992 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9702 _exptl_absorpt_correction_T_max 0.9849 _exptl_absorpt_process_details ; BRUKER AXS SMART APEX 2 Vers. 1.0-27 R.H. Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(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 ? _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 53133 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_sigmaI/netI 0.0777 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 24.77 _reflns_number_total 14249 _reflns_number_gt 8481 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0682P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment calcd _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14249 _refine_ls_number_parameters 943 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0935 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1288 _refine_ls_wR_factor_gt 0.1136 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _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 Mg1 Mg 0.08007(4) 0.77089(3) 0.91183(4) 0.01939(18) Uani 1 1 d . . . Mg2 Mg 0.40616(4) 0.78441(3) 0.87387(4) 0.01802(18) Uani 1 1 d . . . N1 N 0.02109(9) 0.69469(7) 0.91146(9) 0.0195(4) Uani 1 1 d . . . N2 N 0.16042(9) 0.74487(7) 0.99875(9) 0.0194(4) Uani 1 1 d . . . N3 N 0.38936(9) 0.80799(7) 0.96163(9) 0.0192(4) Uani 1 1 d . . . N4 N 0.44257(9) 0.86632(7) 0.85622(9) 0.0190(4) Uani 1 1 d . . . N5 N 0.03272(10) 0.84994(8) 0.92351(9) 0.0216(4) Uani 1 1 d . . . N6 N 0.09377(10) 0.79219(8) 0.82237(9) 0.0197(4) Uani 1 1 d . . . N7 N 0.33110(9) 0.74760(7) 0.78980(9) 0.0191(4) Uani 1 1 d . . . N8 N 0.47800(9) 0.71603(8) 0.87871(9) 0.0194(4) Uani 1 1 d . . . C1 C -0.03879(13) 0.63520(10) 0.97687(12) 0.0288(6) Uani 1 1 d . . . H1A H -0.0785 0.6296 0.9326 0.043 Uiso 1 1 calc R . . H1B H -0.0611 0.6467 1.0110 0.043 Uiso 1 1 calc R . . H1C H -0.0110 0.5986 0.9911 0.043 Uiso 1 1 calc R . . C2 C 0.01390(12) 0.68251(9) 0.97075(11) 0.0202(5) Uani 1 1 d . . . C3 C 0.05734(12) 0.71130(9) 1.03169(11) 0.0203(5) Uani 1 1 d . . . H3 H 0.0350 0.7157 1.0658 0.026 Uiso 1 1 calc R . . C4 C 0.12947(12) 0.73389(9) 1.04702(11) 0.0211(5) Uani 1 1 d . . . C5 C 0.17048(13) 0.74916(10) 1.12130(11) 0.0272(6) Uani 1 1 d . . . H5A H 0.2213 0.7623 1.1269 0.041 Uiso 1 1 calc R . . H5B H 0.1730 0.7145 1.1498 0.041 Uiso 1 1 calc R . . H5C H 0.1436 0.7805 1.1353 0.041 Uiso 1 1 calc R . . C6 C -0.00199(12) 0.65261(9) 0.85705(11) 0.0211(5) Uani 1 1 d . . . C7 C 0.04128(13) 0.60189(10) 0.86280(12) 0.0262(6) Uani 1 1 d . . . C8 C 0.02431(14) 0.56456(11) 0.80674(12) 0.0336(6) Uani 1 1 d . . . H8 H 0.0534 0.5302 0.8096 0.044 Uiso 1 1 calc R . . C9 C -0.03389(14) 0.57661(11) 0.74727(13) 0.0341(6) Uani 1 1 d . . . H9 H -0.0443 0.5508 0.7094 0.044 Uiso 1 1 calc R . . C10 C -0.07687(13) 0.62569(10) 0.74257(12) 0.0283(6) Uani 1 1 d . . . H10 H -0.1176 0.6331 0.7016 0.037 Uiso 1 1 calc R . . C11 C -0.06184(12) 0.66495(10) 0.79690(12) 0.0227(5) Uani 1 1 d . . . C12 C 0.10885(13) 0.58841(10) 0.92647(12) 0.0305(6) Uani 1 1 d . . . H12 H 0.1082 0.6167 0.9629 0.037 Uiso 1 1 calc R . . C13 C 0.18102(14) 0.59812(12) 0.91216(13) 0.0416(7) Uani 1 1 d . . . H13A H 0.1823 0.5721 0.8752 0.062 Uiso 1 1 calc R . . H13B H 0.2238 0.5896 0.9535 0.062 Uiso 1 1 calc R . . H13C H 0.1836 0.6389 0.8986 0.062 Uiso 1 1 calc R . . C14 C 0.10591(16) 0.52663(11) 0.95379(13) 0.0430(7) Uani 1 1 d . . . H14A H 0.0584 0.5211 0.9616 0.064 Uiso 1 1 calc R . . H14B H 0.1476 0.5213 0.9969 0.064 Uiso 1 1 calc R . . H14C H 0.1099 0.4978 0.9203 0.064 Uiso 1 1 calc R . . C15 C -0.11051(14) 0.71829(11) 0.79004(12) 0.0325(6) Uani 1 1 d . . . H15 H -0.0855 0.7444 0.8299 0.039 Uiso 1 1 calc R . . C16 C -0.18707(15) 0.70154(14) 0.79311(16) 0.0591(9) Uani 1 1 d . . . H16A H -0.2125 0.6752 0.7551 0.089 Uiso 1 1 calc R . . H16B H -0.2173 0.7369 0.7897 0.089 Uiso 1 1 calc R . . H16C H -0.1805 0.6817 0.8365 0.089 Uiso 1 1 calc R . . C17 C -0.11905(14) 0.75295(12) 0.72516(14) 0.0414(7) Uani 1 1 d . . . H17A H -0.0694 0.7638 0.7245 0.062 Uiso 1 1 calc R . . H17B H -0.1484 0.7884 0.7243 0.062 Uiso 1 1 calc R . . H17C H -0.1448 0.7289 0.6851 0.062 Uiso 1 1 calc R . . C18 C 0.23893(12) 0.73889(9) 1.01415(11) 0.0182(5) Uani 1 1 d . . . C19 C 0.27844(12) 0.69210(9) 1.05296(11) 0.0216(5) Uani 1 1 d . . . H19 H 0.2538 0.6657 1.0734 0.028 Uiso 1 1 calc R . . C20 C 0.35318(12) 0.68405(10) 1.06180(11) 0.0232(5) Uani 1 1 d . . . H20 H 0.3795 0.6520 1.0883 0.030 Uiso 1 1 calc R . . C21 C 0.39035(12) 0.72213(10) 1.03243(11) 0.0218(5) Uani 1 1 d . . . H21 H 0.4418 0.7162 1.0389 0.028 Uiso 1 1 calc R . . C22 C 0.35197(12) 0.76896(9) 0.99363(11) 0.0185(5) Uani 1 1 d . . . C23 C 0.27638(12) 0.77675(9) 0.98439(11) 0.0189(5) Uani 1 1 d . . . H23 H 0.2499 0.8085 0.9573 0.025 Uiso 1 1 calc R . . C24 C 0.42352(13) 0.86456(10) 1.06847(11) 0.0268(6) Uani 1 1 d . . . H24A H 0.3721 0.8684 1.0684 0.040 Uiso 1 1 calc R . . H24B H 0.4517 0.9002 1.0874 0.040 Uiso 1 1 calc R . . H24C H 0.4477 0.8309 1.0965 0.040 Uiso 1 1 calc R . . C25 C 0.42209(12) 0.85566(9) 0.99599(11) 0.0194(5) Uani 1 1 d . . . C26 C 0.45504(12) 0.89962(9) 0.96932(11) 0.0219(5) Uani 1 1 d . . . H26 H 0.4789 0.9294 1.0011 0.028 Uiso 1 1 calc R . . C27 C 0.45912(12) 0.90763(9) 0.90394(11) 0.0207(5) Uani 1 1 d . . . C28 C 0.48179(14) 0.96838(9) 0.88991(12) 0.0274(6) Uani 1 1 d . . . H28A H 0.4910 0.9684 0.8464 0.041 Uiso 1 1 calc R . . H28B H 0.5275 0.9801 0.9268 0.041 Uiso 1 1 calc R . . H28C H 0.4415 0.9960 0.8873 0.041 Uiso 1 1 calc R . . C29 C 0.44242(12) 0.87980(9) 0.78859(11) 0.0203(5) Uani 1 1 d . . . C30 C 0.50494(13) 0.86409(9) 0.77006(12) 0.0255(6) Uani 1 1 d . . . C31 C 0.50030(15) 0.87259(10) 0.70263(13) 0.0333(6) Uani 1 1 d . . . H31 H 0.5419 0.8624 0.6895 0.043 Uiso 1 1 calc R . . C32 C 0.43708(15) 0.89540(10) 0.65441(13) 0.0365(7) Uani 1 1 d . . . H32 H 0.4348 0.9001 0.6084 0.048 Uiso 1 1 calc R . . C33 C 0.37709(15) 0.91134(10) 0.67356(12) 0.0317(6) Uani 1 1 d . . . H33 H 0.3337 0.9273 0.6402 0.041 Uiso 1 1 calc R . . C34 C 0.37844(13) 0.90473(9) 0.74026(11) 0.0231(5) Uani 1 1 d . . . C35 C 0.57624(13) 0.84018(11) 0.82164(13) 0.0314(6) Uani 1 1 d . . . H35 H 0.5619 0.8152 0.8546 0.038 Uiso 1 1 calc R . . C36 C 0.62647(15) 0.88954(12) 0.86235(15) 0.0491(8) Uani 1 1 d . . . H36A H 0.6336 0.9188 0.8307 0.074 Uiso 1 1 calc R . . H36B H 0.6752 0.8734 0.8901 0.074 Uiso 1 1 calc R . . H36C H 0.6028 0.9080 0.8923 0.074 Uiso 1 1 calc R . . C37 C 0.62179(15) 0.80255(12) 0.78973(14) 0.0422(7) Uani 1 1 d . . . H37A H 0.5887 0.7743 0.7582 0.063 Uiso 1 1 calc R . . H37B H 0.6607 0.7816 0.8258 0.063 Uiso 1 1 calc R . . H37C H 0.6453 0.8276 0.7647 0.063 Uiso 1 1 calc R . . C38 C 0.31213(12) 0.92661(10) 0.75807(12) 0.0263(6) Uani 1 1 d . . . H38 H 0.3211 0.9166 0.8070 0.032 Uiso 1 1 calc R . . C39 C 0.23946(13) 0.89777(11) 0.71473(13) 0.0350(6) Uani 1 1 d . . . H39A H 0.2282 0.9086 0.6667 0.052 Uiso 1 1 calc R . . H39B H 0.1987 0.9109 0.7300 0.052 Uiso 1 1 calc R . . H39C H 0.2446 0.8552 0.7195 0.052 Uiso 1 1 calc R . . C40 C 0.30425(14) 0.99316(10) 0.75038(13) 0.0336(6) Uani 1 1 d . . . H40A H 0.3516 1.0118 0.7773 0.050 Uiso 1 1 calc R . . H40B H 0.2645 1.0066 0.7668 0.050 Uiso 1 1 calc R . . H40C H 0.2916 1.0038 0.7021 0.050 Uiso 1 1 calc R . . C41 C -0.02111(14) 0.94671(10) 0.88044(13) 0.0314(6) Uani 1 1 d . . . H41A H -0.0427 0.9444 0.9168 0.047 Uiso 1 1 calc R . . H41B H -0.0601 0.9581 0.8376 0.047 Uiso 1 1 calc R . . H41C H 0.0191 0.9759 0.8926 0.047 Uiso 1 1 calc R . . C42 C 0.01018(12) 0.88779(10) 0.87168(12) 0.0235(6) Uani 1 1 d . . . C43 C 0.01497(12) 0.87780(10) 0.80677(12) 0.0239(6) Uani 1 1 d . . . H43 H -0.0132 0.9044 0.7725 0.031 Uiso 1 1 calc R . . C44 C 0.05403(12) 0.83546(10) 0.78364(11) 0.0213(5) Uani 1 1 d . . . C45 C 0.05081(13) 0.84065(10) 0.71068(11) 0.0272(6) Uani 1 1 d . . . H45A H 0.1018 0.8434 0.7094 0.041 Uiso 1 1 calc R . . H45B H 0.0227 0.8759 0.6901 0.041 Uiso 1 1 calc R . . H45C H 0.0259 0.8061 0.6850 0.041 Uiso 1 1 calc R . . C46 C 0.02798(13) 0.86674(9) 0.98860(12) 0.0228(5) Uani 1 1 d . . . C47 C 0.08389(13) 0.90082(10) 1.03415(12) 0.0259(6) Uani 1 1 d . . . C48 C 0.07951(14) 0.91240(10) 1.09852(13) 0.0330(6) Uani 1 1 d . . . H48 H 0.1177 0.9350 1.1303 0.043 Uiso 1 1 calc R . . C49 C 0.02117(16) 0.89178(11) 1.11683(14) 0.0382(7) Uani 1 1 d . . . H49 H 0.0188 0.9005 1.1606 0.050 Uiso 1 1 calc R . . C50 C -0.03427(15) 0.85822(10) 1.07087(14) 0.0365(7) Uani 1 1 d . . . H50 H -0.0744 0.8438 1.0838 0.047 Uiso 1 1 calc R . . C51 C -0.03235(13) 0.84537(10) 1.00708(13) 0.0271(6) Uani 1 1 d . . . C52 C 0.14862(13) 0.92696(10) 1.01675(13) 0.0287(6) Uani 1 1 d . . . H52 H 0.1423 0.9158 0.9687 0.034 Uiso 1 1 calc R . . C53 C 0.22377(14) 0.90349(11) 1.06309(14) 0.0385(7) Uani 1 1 d . . . H53A H 0.2304 0.9128 1.1107 0.058 Uiso 1 1 calc R . . H53B H 0.2641 0.9216 1.0508 0.058 Uiso 1 1 calc R . . H53C H 0.2252 0.8610 1.0576 0.058 Uiso 1 1 calc R . . C54 C 0.14986(15) 0.99429(10) 1.02115(14) 0.0380(7) Uani 1 1 d . . . H54A H 0.1011 1.0098 0.9926 0.057 Uiso 1 1 calc R . . H54B H 0.1890 1.0096 1.0050 0.057 Uiso 1 1 calc R . . H54C H 0.1603 1.0063 1.0687 0.057 Uiso 1 1 calc R . . C55 C -0.09447(13) 0.80899(10) 0.95772(13) 0.0321(6) Uani 1 1 d . . . H55 H -0.0707 0.7830 0.9323 0.038 Uiso 1 1 calc R . . C56 C -0.15221(14) 0.84696(12) 0.90462(15) 0.0504(8) Uani 1 1 d . . . H56A H -0.1739 0.8752 0.9280 0.076 Uiso 1 1 calc R . . H56B H -0.1919 0.8220 0.8748 0.076 Uiso 1 1 calc R . . H56C H -0.1277 0.8680 0.8771 0.076 Uiso 1 1 calc R . . C57 C -0.13551(15) 0.76929(12) 0.99264(15) 0.0469(8) Uani 1 1 d . . . H57A H -0.0988 0.7479 1.0301 0.070 Uiso 1 1 calc R . . H57B H -0.1668 0.7414 0.9593 0.070 Uiso 1 1 calc R . . H57C H -0.1671 0.7932 1.0108 0.070 Uiso 1 1 calc R . . C58 C 0.13721(12) 0.75501(9) 0.79417(11) 0.0179(5) Uani 1 1 d . . . C59 C 0.10685(12) 0.70370(10) 0.76052(11) 0.0223(5) Uani 1 1 d . . . H59 H 0.0566 0.6934 0.7545 0.029 Uiso 1 1 calc R . . C60 C 0.14997(12) 0.66753(10) 0.73582(11) 0.0231(5) Uani 1 1 d . . . H60 H 0.1292 0.6322 0.7133 0.030 Uiso 1 1 calc R . . C61 C 0.22310(12) 0.68223(9) 0.74359(11) 0.0213(5) Uani 1 1 d . . . H61 H 0.2521 0.6570 0.7263 0.028 Uiso 1 1 calc R . . C62 C 0.25426(11) 0.73366(9) 0.77650(10) 0.0177(5) Uani 1 1 d . . . C63 C 0.21091(12) 0.76955(9) 0.80240(11) 0.0180(5) Uani 1 1 d . . . H63 H 0.2320 0.8044 0.8260 0.023 Uiso 1 1 calc R . . C64 C 0.31618(12) 0.74273(10) 0.66658(11) 0.0237(5) Uani 1 1 d . . . H64A H 0.3081 0.7038 0.6455 0.036 Uiso 1 1 calc R . . H64B H 0.3430 0.7674 0.6441 0.036 Uiso 1 1 calc R . . H64C H 0.2677 0.7606 0.6615 0.036 Uiso 1 1 calc R . . C65 C 0.36206(12) 0.73717(9) 0.74168(11) 0.0187(5) Uani 1 1 d . . . C66 C 0.43741(12) 0.72291(9) 0.75695(11) 0.0206(5) Uani 1 1 d . . . H66 H 0.4574 0.7274 0.7212 0.027 Uiso 1 1 calc R . . C67 C 0.48722(12) 0.70235(9) 0.82065(11) 0.0194(5) Uani 1 1 d . . . C68 C 0.54900(13) 0.66174(10) 0.81862(12) 0.0297(6) Uani 1 1 d . . . H68A H 0.5922 0.6661 0.8607 0.045 Uiso 1 1 calc R . . H68B H 0.5638 0.6715 0.7792 0.045 Uiso 1 1 calc R . . H68C H 0.5311 0.6212 0.8146 0.045 Uiso 1 1 calc R . . C69 C 0.51126(12) 0.68042(9) 0.93825(11) 0.0206(5) Uani 1 1 d . . . C70 C 0.48283(12) 0.62370(10) 0.93929(11) 0.0230(5) Uani 1 1 d . . . C71 C 0.51016(13) 0.59242(10) 0.99968(12) 0.0293(6) Uani 1 1 d . . . H71 H 0.4913 0.5542 1.0016 0.038 Uiso 1 1 calc R . . C72 C 0.56416(13) 0.61496(10) 1.05739(12) 0.0284(6) Uani 1 1 d . . . H72 H 0.5824 0.5923 1.0980 0.037 Uiso 1 1 calc R . . C73 C 0.59123(13) 0.67079(10) 1.05531(12) 0.0270(6) Uani 1 1 d . . . H73 H 0.6284 0.6863 1.0948 0.035 Uiso 1 1 calc R . . C74 C 0.56511(12) 0.70450(10) 0.99658(11) 0.0214(5) Uani 1 1 d . . . C75 C 0.42054(13) 0.59840(10) 0.87908(12) 0.0275(6) Uani 1 1 d . . . H75 H 0.4163 0.6227 0.8380 0.033 Uiso 1 1 calc R . . C76 C 0.34615(14) 0.60251(12) 0.89207(13) 0.0424(7) Uani 1 1 d . . . H76A H 0.3486 0.5783 0.9316 0.064 Uiso 1 1 calc R . . H76B H 0.3055 0.5886 0.8517 0.064 Uiso 1 1 calc R . . H76C H 0.3368 0.6433 0.9012 0.064 Uiso 1 1 calc R . . C77 C 0.43579(17) 0.53530(10) 0.86351(14) 0.0474(8) Uani 1 1 d . . . H77A H 0.4845 0.5331 0.8572 0.071 Uiso 1 1 calc R . . H77B H 0.3964 0.5222 0.8217 0.071 Uiso 1 1 calc R . . H77C H 0.4363 0.5100 0.9017 0.071 Uiso 1 1 calc R . . C78 C 0.59497(12) 0.76594(10) 0.99660(12) 0.0257(6) Uani 1 1 d . . . H78 H 0.5583 0.7877 0.9578 0.031 Uiso 1 1 calc R . . C79 C 0.60339(13) 0.79955(10) 1.06193(12) 0.0314(6) Uani 1 1 d . . . H79A H 0.5571 0.7962 1.0724 0.047 Uiso 1 1 calc R . . H79B H 0.6133 0.8408 1.0557 0.047 Uiso 1 1 calc R . . H79C H 0.6452 0.7832 1.0997 0.047 Uiso 1 1 calc R . . C80 C 0.66944(13) 0.76417(11) 0.98371(13) 0.0365(7) Uani 1 1 d . . . H80A H 0.7065 0.7426 1.0207 0.055 Uiso 1 1 calc R . . H80B H 0.6873 0.8042 0.9821 0.055 Uiso 1 1 calc R . . H80C H 0.6623 0.7446 0.9401 0.055 Uiso 1 1 calc R . . C81 C 0.7181(3) 0.5690(2) 0.8798(2) 0.0962(16) Uani 1 1 d . . . H81 H 0.7287 0.5792 0.8399 0.125 Uiso 1 1 calc R . . C82 C 0.6823(3) 0.5164(2) 0.8826(2) 0.0948(15) Uani 1 1 d . . . H82 H 0.6681 0.4904 0.8447 0.123 Uiso 1 1 calc R . . C83 C 0.6677(2) 0.50267(16) 0.9419(2) 0.0724(10) Uani 1 1 d . . . H83 H 0.6435 0.4669 0.9451 0.094 Uiso 1 1 calc R . . C84 C 0.68816(19) 0.54069(15) 0.99534(18) 0.0616(9) Uani 1 1 d . . . H84 H 0.6782 0.5314 1.0359 0.080 Uiso 1 1 calc R . . C85 C 0.72283(18) 0.59196(15) 0.99115(19) 0.0630(9) Uani 1 1 d . . . H85 H 0.7365 0.6184 1.0286 0.082 Uiso 1 1 calc R . . C86 C 0.73777(19) 0.60534(18) 0.9344(2) 0.0759(11) Uani 1 1 d . . . H86 H 0.7626 0.6410 0.9325 0.099 Uiso 1 1 calc R . . C87 C 0.70820(15) 0.97392(13) 0.07665(14) 0.0441(7) Uani 1 1 d . . . H87 H 0.6585 0.9663 0.0471 0.057 Uiso 1 1 calc R . . C88 C 0.75599(15) 0.92748(12) 0.10597(14) 0.0407(7) Uani 1 1 d . . . H88 H 0.7393 0.8882 0.0962 0.053 Uiso 1 1 calc R . . C89 C 0.82758(14) 0.93903(12) 0.14922(13) 0.0371(7) Uani 1 1 d . . . H89 H 0.8603 0.9076 0.1698 0.048 Uiso 1 1 calc R . . C90 C 0.85199(15) 0.99610(12) 0.16286(13) 0.0365(7) Uani 1 1 d . . . H90 H 0.9015 1.0039 0.1927 0.047 Uiso 1 1 calc R . . C91 C 0.80469(16) 1.04166(12) 0.13333(14) 0.0381(7) Uani 1 1 d . . . H91 H 0.8218 1.0809 0.1427 0.050 Uiso 1 1 calc R . . C92 C 0.73278(16) 1.03086(12) 0.09032(14) 0.0408(7) Uani 1 1 d . . . H92 H 0.7002 1.0624 0.0701 0.053 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 Mg1 0.0194(4) 0.0187(4) 0.0204(4) 0.0008(3) 0.0071(3) 0.0013(3) Mg2 0.0184(4) 0.0182(4) 0.0162(4) -0.0015(3) 0.0044(3) -0.0009(3) N1 0.0168(10) 0.0200(10) 0.0197(11) 0.0005(9) 0.0037(9) 0.0009(8) N2 0.0198(10) 0.0198(10) 0.0175(11) 0.0008(8) 0.0051(9) -0.0009(8) N3 0.0182(10) 0.0189(10) 0.0189(11) -0.0014(8) 0.0045(9) -0.0029(8) N4 0.0200(10) 0.0179(10) 0.0186(11) -0.0008(9) 0.0059(9) 0.0004(8) N5 0.0203(10) 0.0209(10) 0.0257(12) 0.0021(9) 0.0108(9) 0.0007(8) N6 0.0171(10) 0.0203(10) 0.0218(11) 0.0012(9) 0.0066(9) 0.0016(8) N7 0.0170(10) 0.0210(10) 0.0185(11) -0.0001(8) 0.0051(9) 0.0011(8) N8 0.0186(10) 0.0202(10) 0.0155(11) 0.0009(8) 0.0008(9) -0.0011(8) C1 0.0273(14) 0.0296(14) 0.0292(15) 0.0009(12) 0.0093(12) -0.0073(11) C2 0.0190(12) 0.0205(12) 0.0215(14) 0.0035(10) 0.0074(11) 0.0044(10) C3 0.0204(12) 0.0224(13) 0.0205(13) -0.0004(10) 0.0103(11) 0.0013(10) C4 0.0251(13) 0.0166(12) 0.0219(14) 0.0029(10) 0.0086(11) 0.0023(10) C5 0.0278(13) 0.0326(14) 0.0209(14) -0.0001(11) 0.0080(12) -0.0024(11) C6 0.0212(13) 0.0214(13) 0.0208(14) -0.0003(11) 0.0076(11) -0.0064(10) C7 0.0265(14) 0.0242(14) 0.0231(14) -0.0032(11) 0.0023(12) 0.0001(11) C8 0.0363(16) 0.0284(14) 0.0291(16) -0.0054(12) 0.0023(13) 0.0043(12) C9 0.0416(16) 0.0304(15) 0.0256(15) -0.0092(12) 0.0054(14) -0.0010(13) C10 0.0258(14) 0.0315(15) 0.0228(14) 0.0010(12) 0.0023(12) -0.0064(11) C11 0.0201(13) 0.0263(13) 0.0215(14) 0.0033(11) 0.0069(11) -0.0038(11) C12 0.0310(14) 0.0288(14) 0.0243(15) -0.0063(11) -0.0001(12) 0.0068(12) C13 0.0329(15) 0.0499(18) 0.0337(16) -0.0088(14) 0.0008(13) 0.0083(13) C14 0.0532(18) 0.0307(16) 0.0336(16) 0.0006(13) 0.0001(14) 0.0101(14) C15 0.0328(15) 0.0350(15) 0.0220(14) 0.0004(12) -0.0006(12) 0.0072(12) C16 0.0462(19) 0.084(2) 0.056(2) 0.0324(18) 0.0296(17) 0.0302(17) C17 0.0278(15) 0.0381(16) 0.0482(18) 0.0126(14) 0.0002(14) 0.0001(12) C18 0.0168(12) 0.0201(12) 0.0159(12) -0.0044(10) 0.0031(10) -0.0013(10) C19 0.0244(13) 0.0220(13) 0.0187(13) -0.0003(10) 0.0077(11) -0.0016(11) C20 0.0261(13) 0.0202(13) 0.0212(14) 0.0025(10) 0.0054(11) 0.0047(11) C21 0.0179(12) 0.0276(13) 0.0176(13) -0.0017(11) 0.0032(10) 0.0006(11) C22 0.0205(12) 0.0217(12) 0.0117(12) -0.0040(10) 0.0037(10) -0.0019(10) C23 0.0193(12) 0.0196(12) 0.0150(12) -0.0011(10) 0.0021(10) 0.0013(10) C24 0.0268(14) 0.0283(14) 0.0229(14) -0.0067(11) 0.0054(11) -0.0055(11) C25 0.0182(12) 0.0216(13) 0.0161(13) -0.0029(10) 0.0031(10) 0.0011(10) C26 0.0228(13) 0.0211(13) 0.0192(13) -0.0045(10) 0.0039(11) -0.0038(10) C27 0.0153(12) 0.0201(13) 0.0230(14) -0.0012(11) 0.0019(11) 0.0000(10) C28 0.0357(15) 0.0219(13) 0.0261(14) -0.0041(11) 0.0124(12) -0.0058(11) C29 0.0281(13) 0.0146(12) 0.0184(13) -0.0007(10) 0.0086(11) -0.0049(10) C30 0.0313(14) 0.0191(13) 0.0303(15) 0.0009(11) 0.0161(12) -0.0003(11) C31 0.0467(17) 0.0288(14) 0.0348(16) 0.0042(12) 0.0274(14) 0.0065(13) C32 0.0608(19) 0.0304(15) 0.0264(15) 0.0064(12) 0.0252(15) 0.0088(14) C33 0.0428(16) 0.0265(14) 0.0234(15) 0.0044(11) 0.0084(13) 0.0034(12) C34 0.0314(14) 0.0175(12) 0.0199(14) -0.0001(10) 0.0079(12) -0.0006(11) C35 0.0270(14) 0.0327(15) 0.0390(16) 0.0028(12) 0.0171(13) 0.0012(12) C36 0.0359(16) 0.0519(19) 0.057(2) -0.0027(16) 0.0130(15) -0.0002(14) C37 0.0383(16) 0.0412(17) 0.0527(19) 0.0061(14) 0.0226(15) 0.0076(13) C38 0.0256(13) 0.0275(14) 0.0232(14) 0.0053(11) 0.0049(12) 0.0008(11) C39 0.0315(15) 0.0340(15) 0.0328(15) 0.0060(12) 0.0026(13) -0.0044(12) C40 0.0379(15) 0.0279(14) 0.0357(16) 0.0044(12) 0.0136(13) 0.0013(12) C41 0.0299(14) 0.0278(14) 0.0387(16) 0.0048(12) 0.0148(13) 0.0106(11) C42 0.0162(12) 0.0223(13) 0.0309(15) 0.0022(11) 0.0067(11) 0.0000(10) C43 0.0202(13) 0.0243(13) 0.0241(14) 0.0059(11) 0.0035(11) 0.0042(10) C44 0.0169(12) 0.0215(13) 0.0224(14) 0.0031(11) 0.0026(11) -0.0018(10) C45 0.0254(13) 0.0309(14) 0.0231(14) 0.0074(11) 0.0055(11) 0.0042(11) C46 0.0282(14) 0.0153(12) 0.0277(14) 0.0041(11) 0.0131(12) 0.0065(11) C47 0.0317(14) 0.0208(13) 0.0289(15) -0.0002(11) 0.0151(12) 0.0047(11) C48 0.0427(16) 0.0239(14) 0.0363(16) -0.0020(12) 0.0186(14) 0.0027(12) C49 0.0594(19) 0.0306(15) 0.0361(17) 0.0018(13) 0.0310(15) 0.0082(14) C50 0.0459(17) 0.0266(14) 0.0489(18) -0.0001(13) 0.0315(15) 0.0006(13) C51 0.0288(14) 0.0225(13) 0.0357(16) 0.0001(11) 0.0184(12) 0.0038(11) C52 0.0314(14) 0.0267(14) 0.0309(15) -0.0059(11) 0.0144(12) -0.0017(11) C53 0.0354(16) 0.0353(16) 0.0439(17) -0.0080(13) 0.0125(14) -0.0011(13) C54 0.0440(16) 0.0291(15) 0.0479(18) -0.0049(13) 0.0248(15) 0.0008(13) C55 0.0276(14) 0.0292(14) 0.0451(17) 0.0003(12) 0.0198(13) 0.0001(12) C56 0.0275(15) 0.0402(17) 0.077(2) 0.0053(16) 0.0103(16) 0.0041(13) C57 0.0436(17) 0.0407(17) 0.069(2) 0.0006(15) 0.0350(16) -0.0030(14) C58 0.0200(12) 0.0195(12) 0.0111(12) 0.0030(10) 0.0013(10) 0.0037(10) C59 0.0206(12) 0.0263(13) 0.0190(13) 0.0015(11) 0.0054(11) -0.0032(11) C60 0.0246(13) 0.0233(13) 0.0199(13) -0.0016(10) 0.0057(11) -0.0048(11) C61 0.0259(13) 0.0225(13) 0.0149(13) -0.0020(10) 0.0064(11) -0.0003(11) C62 0.0165(12) 0.0217(13) 0.0113(12) 0.0009(10) 0.0002(10) -0.0010(10) C63 0.0206(12) 0.0173(12) 0.0149(12) -0.0010(10) 0.0044(10) -0.0032(10) C64 0.0215(13) 0.0311(14) 0.0165(13) 0.0000(11) 0.0039(11) -0.0001(11) C65 0.0224(13) 0.0149(12) 0.0191(13) -0.0004(10) 0.0076(11) -0.0021(10) C66 0.0225(13) 0.0226(13) 0.0177(13) -0.0018(10) 0.0084(11) 0.0002(10) C67 0.0191(12) 0.0208(12) 0.0168(14) -0.0025(10) 0.0044(11) -0.0023(10) C68 0.0246(13) 0.0346(15) 0.0275(15) -0.0007(12) 0.0060(12) 0.0094(11) C69 0.0195(12) 0.0228(13) 0.0182(13) 0.0011(11) 0.0050(11) 0.0058(10) C70 0.0240(13) 0.0222(13) 0.0197(13) -0.0018(11) 0.0035(11) 0.0018(10) C71 0.0312(14) 0.0230(13) 0.0274(15) 0.0029(12) 0.0022(13) 0.0002(11) C72 0.0288(14) 0.0299(14) 0.0211(14) 0.0048(11) 0.0018(12) 0.0040(12) C73 0.0231(13) 0.0323(14) 0.0195(14) -0.0027(11) -0.0006(11) -0.0004(11) C74 0.0168(12) 0.0257(13) 0.0192(14) -0.0009(11) 0.0027(11) 0.0023(10) C75 0.0316(14) 0.0226(13) 0.0205(14) 0.0016(11) -0.0010(12) -0.0046(11) C76 0.0390(16) 0.0471(18) 0.0333(16) 0.0047(13) 0.0024(14) -0.0121(14) C77 0.062(2) 0.0267(15) 0.0342(17) -0.0022(13) -0.0084(15) -0.0022(14) C78 0.0207(13) 0.0290(14) 0.0226(14) -0.0001(11) 0.0011(11) -0.0004(11) C79 0.0261(14) 0.0307(14) 0.0303(15) -0.0050(12) 0.0005(12) 0.0016(11) C80 0.0272(14) 0.0437(17) 0.0374(16) -0.0007(13) 0.0098(13) -0.0058(12) C81 0.120(4) 0.102(4) 0.093(4) 0.041(3) 0.070(3) 0.068(3) C82 0.121(4) 0.096(4) 0.058(3) -0.008(3) 0.018(3) 0.067(3) C83 0.069(2) 0.057(2) 0.087(3) -0.004(2) 0.023(2) 0.0136(19) C84 0.069(2) 0.056(2) 0.069(2) 0.008(2) 0.036(2) 0.0180(19) C85 0.061(2) 0.056(2) 0.065(2) 0.0104(19) 0.0121(19) 0.0159(18) C86 0.056(2) 0.082(3) 0.100(3) 0.032(3) 0.040(2) 0.024(2) C87 0.0320(16) 0.064(2) 0.0358(17) 0.0033(15) 0.0117(14) -0.0009(15) C88 0.0400(17) 0.0371(16) 0.0464(18) -0.0018(14) 0.0168(15) -0.0064(14) C89 0.0331(16) 0.0366(16) 0.0424(18) 0.0050(13) 0.0140(14) 0.0039(13) C90 0.0327(15) 0.0417(17) 0.0391(17) -0.0035(14) 0.0173(14) -0.0051(14) C91 0.0473(18) 0.0363(16) 0.0406(17) -0.0007(13) 0.0279(15) -0.0044(14) C92 0.0450(18) 0.0438(18) 0.0408(18) 0.0131(14) 0.0241(15) 0.0135(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 N2 2.0171(19) . ? Mg1 N6 2.0278(19) . ? Mg1 N5 2.0698(19) . ? Mg1 N1 2.0700(19) . ? Mg1 C4 2.777(2) . ? Mg1 C2 2.869(2) . ? Mg2 N7 2.0242(19) . ? Mg2 N3 2.0335(19) . ? Mg2 N8 2.0551(19) . ? Mg2 N4 2.0723(19) . ? Mg2 C65 2.805(2) . ? N1 C2 1.318(3) . ? N1 C6 1.436(3) . ? N2 C4 1.351(3) . ? N2 C18 1.422(3) . ? N3 C25 1.335(3) . ? N3 C22 1.439(3) . ? N4 C27 1.328(3) . ? N4 C29 1.441(3) . ? N5 C42 1.334(3) . ? N5 C46 1.442(3) . ? N6 C44 1.335(3) . ? N6 C58 1.443(3) . ? N7 C65 1.346(3) . ? N7 C62 1.427(3) . ? N8 C67 1.318(3) . ? N8 C69 1.436(3) . ? C1 C2 1.509(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.417(3) . ? C3 C4 1.396(3) . ? C3 H3 0.9500 . ? C4 C5 1.515(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C11 1.402(3) . ? C6 C7 1.403(3) . ? C7 C8 1.392(3) . ? C7 C12 1.528(3) . ? C8 C9 1.377(3) . ? C8 H8 0.9500 . ? C9 C10 1.371(3) . ? C9 H9 0.9500 . ? C10 C11 1.395(3) . ? C10 H10 0.9500 . ? C11 C15 1.507(3) . ? C12 C13 1.517(3) . ? C12 C14 1.531(3) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.526(3) . ? C15 C16 1.528(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 C23 1.394(3) . ? C18 C19 1.395(3) . ? C19 C20 1.381(3) . ? C19 H19 0.9500 . ? C20 C21 1.388(3) . ? C20 H20 0.9500 . ? C21 C22 1.388(3) . ? C21 H21 0.9500 . ? C22 C23 1.394(3) . ? C23 H23 0.9500 . ? C24 C25 1.515(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.396(3) . ? C26 C27 1.403(3) . ? C26 H26 0.9500 . ? C27 C28 1.512(3) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C34 1.406(3) . ? C29 C30 1.416(3) . ? C30 C31 1.391(3) . ? C30 C35 1.514(3) . ? C31 C32 1.378(3) . ? C31 H31 0.9500 . ? C32 C33 1.380(3) . ? C32 H32 0.9500 . ? C33 C34 1.389(3) . ? C33 H33 0.9500 . ? C34 C38 1.516(3) . ? C35 C37 1.525(3) . ? C35 C36 1.532(4) . ? C35 H35 1.0000 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.518(3) . ? C38 C40 1.532(3) . ? C38 H38 1.0000 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.509(3) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.405(3) . ? C43 C44 1.402(3) . ? C43 H43 0.9500 . ? C44 C45 1.505(3) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.395(3) . ? C46 C51 1.416(3) . ? C47 C48 1.397(3) . ? C47 C52 1.520(3) . ? C48 C49 1.374(3) . ? C48 H48 0.9500 . ? C49 C50 1.387(4) . ? C49 H49 0.9500 . ? C50 C51 1.374(3) . ? C50 H50 0.9500 . ? C51 C55 1.520(3) . ? C52 C53 1.521(3) . ? C52 C54 1.541(3) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.533(3) . ? C55 C57 1.533(3) . ? C55 H55 1.0000 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C59 1.386(3) . ? C58 C63 1.392(3) . ? C59 C60 1.382(3) . ? C59 H59 0.9500 . ? C60 C61 1.385(3) . ? C60 H60 0.9500 . ? C61 C62 1.387(3) . ? C61 H61 0.9500 . ? C62 C63 1.396(3) . ? C63 H63 0.9500 . ? C64 C65 1.513(3) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C66 1.395(3) . ? C66 C67 1.420(3) . ? C66 H66 0.9500 . ? C67 C68 1.509(3) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 C74 1.405(3) . ? C69 C70 1.408(3) . ? C70 C71 1.384(3) . ? C70 C75 1.514(3) . ? C71 C72 1.385(3) . ? C71 H71 0.9500 . ? C72 C73 1.382(3) . ? C72 H72 0.9500 . ? C73 C74 1.386(3) . ? C73 H73 0.9500 . ? C74 C78 1.515(3) . ? C75 C77 1.528(3) . ? C75 C76 1.531(3) . ? C75 H75 1.0000 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 C79 1.523(3) . ? C78 C80 1.529(3) . ? C78 H78 1.0000 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 C86 1.354(6) . ? C81 C82 1.391(6) . ? C81 H81 0.9500 . ? C82 C83 1.393(5) . ? C82 H82 0.9500 . ? C83 C84 1.359(5) . ? C83 H83 0.9500 . ? C84 C85 1.362(4) . ? C84 H84 0.9500 . ? C85 C86 1.343(5) . ? C85 H85 0.9500 . ? C86 H86 0.9500 . ? C87 C92 1.379(4) . ? C87 C88 1.394(4) . ? C87 H87 0.9500 . ? C88 C89 1.376(3) . ? C88 H88 0.9500 . ? C89 C90 1.381(3) . ? C89 H89 0.9500 . ? C90 C91 1.376(4) . ? C90 H90 0.9500 . ? C91 C92 1.376(4) . ? C91 H91 0.9500 . ? C92 H92 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Mg1 N6 126.83(8) . . ? N2 Mg1 N5 112.20(8) . . ? N6 Mg1 N5 95.54(8) . . ? N2 Mg1 N1 89.88(7) . . ? N6 Mg1 N1 116.02(8) . . ? N5 Mg1 N1 118.56(7) . . ? N2 Mg1 C4 27.30(6) . . ? N6 Mg1 C4 154.12(7) . . ? N5 Mg1 C4 98.98(7) . . ? N1 Mg1 C4 75.05(7) . . ? N2 Mg1 C2 73.53(7) . . ? N6 Mg1 C2 140.88(7) . . ? N5 Mg1 C2 106.99(7) . . ? N1 Mg1 C2 24.86(6) . . ? C4 Mg1 C2 52.93(6) . . ? N7 Mg2 N3 127.34(8) . . ? N7 Mg2 N8 89.19(7) . . ? N3 Mg2 N8 117.65(8) . . ? N7 Mg2 N4 113.65(8) . . ? N3 Mg2 N4 94.88(7) . . ? N8 Mg2 N4 116.04(7) . . ? N7 Mg2 C65 26.61(6) . . ? N3 Mg2 C65 153.95(7) . . ? N8 Mg2 C65 74.06(7) . . ? N4 Mg2 C65 100.31(7) . . ? C2 N1 C6 119.77(18) . . ? C2 N1 Mg1 113.84(14) . . ? C6 N1 Mg1 125.82(14) . . ? C4 N2 C18 120.37(18) . . ? C4 N2 Mg1 109.49(14) . . ? C18 N2 Mg1 130.11(14) . . ? C25 N3 C22 118.11(18) . . ? C25 N3 Mg2 120.70(14) . . ? C22 N3 Mg2 120.47(13) . . ? C27 N4 C29 120.02(18) . . ? C27 N4 Mg2 121.14(14) . . ? C29 N4 Mg2 118.54(13) . . ? C42 N5 C46 118.83(18) . . ? C42 N5 Mg1 120.18(15) . . ? C46 N5 Mg1 120.86(14) . . ? C44 N6 C58 118.33(18) . . ? C44 N6 Mg1 120.59(14) . . ? C58 N6 Mg1 120.31(14) . . ? C65 N7 C62 119.74(18) . . ? C65 N7 Mg2 111.06(13) . . ? C62 N7 Mg2 129.19(14) . . ? C67 N8 C69 120.03(18) . . ? C67 N8 Mg2 115.51(14) . . ? C69 N8 Mg2 124.17(14) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 121.7(2) . . ? N1 C2 C1 121.0(2) . . ? C3 C2 C1 117.19(19) . . ? N1 C2 Mg1 41.30(10) . . ? C3 C2 Mg1 81.37(13) . . ? C1 C2 Mg1 160.41(16) . . ? C4 C3 C2 127.0(2) . . ? C4 C3 H3 116.5 . . ? C2 C3 H3 116.5 . . ? N2 C4 C3 122.9(2) . . ? N2 C4 C5 120.95(19) . . ? C3 C4 C5 116.1(2) . . ? N2 C4 Mg1 43.21(10) . . ? C3 C4 Mg1 85.22(14) . . ? C5 C4 Mg1 147.34(15) . . ? 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 . . ? C11 C6 C7 121.0(2) . . ? C11 C6 N1 120.4(2) . . ? C7 C6 N1 118.35(19) . . ? C8 C7 C6 118.3(2) . . ? C8 C7 C12 119.2(2) . . ? C6 C7 C12 122.3(2) . . ? C9 C8 C7 121.1(2) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C10 C9 C8 120.2(2) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 121.1(2) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C10 C11 C6 118.2(2) . . ? C10 C11 C15 119.7(2) . . ? C6 C11 C15 122.1(2) . . ? C13 C12 C7 110.3(2) . . ? C13 C12 C14 111.0(2) . . ? C7 C12 C14 112.4(2) . . ? C13 C12 H12 107.6 . . ? C7 C12 H12 107.6 . . ? C14 C12 H12 107.6 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C17 112.3(2) . . ? C11 C15 C16 110.9(2) . . ? C17 C15 C16 110.7(2) . . ? C11 C15 H15 107.6 . . ? C17 C15 H15 107.6 . . ? C16 C15 H15 107.6 . . ? 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 . . ? C23 C18 C19 118.56(19) . . ? C23 C18 N2 119.79(19) . . ? C19 C18 N2 121.31(19) . . ? C20 C19 C18 120.3(2) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 120.9(2) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C22 C21 C20 119.6(2) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C23 119.3(2) . . ? C21 C22 N3 120.21(19) . . ? C23 C22 N3 120.43(19) . . ? C18 C23 C22 121.3(2) . . ? C18 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C25 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C25 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C25 C26 124.4(2) . . ? N3 C25 C24 119.34(19) . . ? C26 C25 C24 116.29(19) . . ? C25 C26 C27 131.5(2) . . ? C25 C26 H26 114.3 . . ? C27 C26 H26 114.3 . . ? N4 C27 C26 123.8(2) . . ? N4 C27 C28 121.2(2) . . ? C26 C27 C28 114.96(19) . . ? 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 . . ? C34 C29 C30 120.6(2) . . ? C34 C29 N4 119.84(19) . . ? C30 C29 N4 119.5(2) . . ? C31 C30 C29 118.1(2) . . ? C31 C30 C35 119.9(2) . . ? C29 C30 C35 121.9(2) . . ? C32 C31 C30 121.8(2) . . ? C32 C31 H31 119.1 . . ? C30 C31 H31 119.1 . . ? C31 C32 C33 119.3(2) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? C32 C33 C34 121.8(2) . . ? C32 C33 H33 119.1 . . ? C34 C33 H33 119.1 . . ? C33 C34 C29 118.4(2) . . ? C33 C34 C38 118.5(2) . . ? C29 C34 C38 123.1(2) . . ? C30 C35 C37 113.5(2) . . ? C30 C35 C36 111.3(2) . . ? C37 C35 C36 108.5(2) . . ? C30 C35 H35 107.8 . . ? C37 C35 H35 107.8 . . ? C36 C35 H35 107.8 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 C39 112.03(19) . . ? C34 C38 C40 111.21(19) . . ? C39 C38 C40 109.44(19) . . ? C34 C38 H38 108.0 . . ? C39 C38 H38 108.0 . . ? C40 C38 H38 108.0 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N5 C42 C43 124.4(2) . . ? N5 C42 C41 120.8(2) . . ? C43 C42 C41 114.8(2) . . ? C44 C43 C42 131.3(2) . . ? C44 C43 H43 114.4 . . ? C42 C43 H43 114.4 . . ? N6 C44 C43 124.1(2) . . ? N6 C44 C45 119.17(19) . . ? C43 C44 C45 116.7(2) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C47 C46 C51 120.5(2) . . ? C47 C46 N5 120.65(19) . . ? C51 C46 N5 118.8(2) . . ? C46 C47 C48 118.5(2) . . ? C46 C47 C52 123.2(2) . . ? C48 C47 C52 118.3(2) . . ? C49 C48 C47 121.4(2) . . ? C49 C48 H48 119.3 . . ? C47 C48 H48 119.3 . . ? C48 C49 C50 119.5(2) . . ? C48 C49 H49 120.2 . . ? C50 C49 H49 120.2 . . ? C51 C50 C49 121.3(2) . . ? C51 C50 H50 119.3 . . ? C49 C50 H50 119.3 . . ? C50 C51 C46 118.8(2) . . ? C50 C51 C55 119.9(2) . . ? C46 C51 C55 121.2(2) . . ? C47 C52 C53 111.8(2) . . ? C47 C52 C54 112.06(19) . . ? C53 C52 C54 108.8(2) . . ? C47 C52 H52 108.0 . . ? C53 C52 H52 108.0 . . ? C54 C52 H52 108.0 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C51 C55 C56 112.1(2) . . ? C51 C55 C57 114.0(2) . . ? C56 C55 C57 108.8(2) . . ? C51 C55 H55 107.2 . . ? C56 C55 H55 107.2 . . ? C57 C55 H55 107.2 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C59 C58 C63 119.4(2) . . ? C59 C58 N6 120.46(19) . . ? C63 C58 N6 120.10(19) . . ? C60 C59 C58 119.8(2) . . ? C60 C59 H59 120.1 . . ? C58 C59 H59 120.1 . . ? C59 C60 C61 120.8(2) . . ? C59 C60 H60 119.6 . . ? C61 C60 H60 119.6 . . ? C60 C61 C62 120.3(2) . . ? C60 C61 H61 119.8 . . ? C62 C61 H61 119.8 . . ? C61 C62 C63 118.7(2) . . ? C61 C62 N7 121.36(19) . . ? C63 C62 N7 119.66(19) . . ? C58 C63 C62 121.0(2) . . ? C58 C63 H63 119.5 . . ? C62 C63 H63 119.5 . . ? C65 C64 H64A 109.5 . . ? C65 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C65 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N7 C65 C66 123.3(2) . . ? N7 C65 C64 120.73(19) . . ? C66 C65 C64 115.98(19) . . ? N7 C65 Mg2 42.33(10) . . ? C66 C65 Mg2 85.89(13) . . ? C64 C65 Mg2 148.78(15) . . ? C65 C66 C67 126.4(2) . . ? C65 C66 H66 116.8 . . ? C67 C66 H66 116.8 . . ? N8 C67 C66 121.54(19) . . ? N8 C67 C68 121.4(2) . . ? C66 C67 C68 116.95(19) . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C74 C69 C70 121.1(2) . . ? C74 C69 N8 119.96(19) . . ? C70 C69 N8 118.53(19) . . ? C71 C70 C69 117.6(2) . . ? C71 C70 C75 119.9(2) . . ? C69 C70 C75 122.3(2) . . ? C70 C71 C72 122.2(2) . . ? C70 C71 H71 118.9 . . ? C72 C71 H71 118.9 . . ? C73 C72 C71 119.3(2) . . ? C73 C72 H72 120.3 . . ? C71 C72 H72 120.3 . . ? C72 C73 C74 121.1(2) . . ? C72 C73 H73 119.5 . . ? C74 C73 H73 119.5 . . ? C73 C74 C69 118.7(2) . . ? C73 C74 C78 119.6(2) . . ? C69 C74 C78 121.7(2) . . ? C70 C75 C77 112.6(2) . . ? C70 C75 C76 109.73(19) . . ? C77 C75 C76 110.5(2) . . ? C70 C75 H75 107.9 . . ? C77 C75 H75 107.9 . . ? C76 C75 H75 107.9 . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C75 C77 H77A 109.5 . . ? C75 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C75 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C74 C78 C79 113.11(19) . . ? C74 C78 C80 110.17(19) . . ? C79 C78 C80 110.51(19) . . ? C74 C78 H78 107.6 . . ? C79 C78 H78 107.6 . . ? C80 C78 H78 107.6 . . ? C78 C79 H79A 109.5 . . ? C78 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C78 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C78 C80 H80A 109.5 . . ? C78 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C78 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C86 C81 C82 119.5(4) . . ? C86 C81 H81 120.2 . . ? C82 C81 H81 120.2 . . ? C81 C82 C83 118.8(4) . . ? C81 C82 H82 120.6 . . ? C83 C82 H82 120.6 . . ? C84 C83 C82 119.6(4) . . ? C84 C83 H83 120.2 . . ? C82 C83 H83 120.2 . . ? C83 C84 C85 120.5(3) . . ? C83 C84 H84 119.8 . . ? C85 C84 H84 119.8 . . ? C86 C85 C84 120.4(4) . . ? C86 C85 H85 119.8 . . ? C84 C85 H85 119.8 . . ? C85 C86 C81 121.3(4) . . ? C85 C86 H86 119.4 . . ? C81 C86 H86 119.4 . . ? C92 C87 C88 120.3(3) . . ? C92 C87 H87 119.9 . . ? C88 C87 H87 119.9 . . ? C89 C88 C87 119.4(3) . . ? C89 C88 H88 120.3 . . ? C87 C88 H88 120.3 . . ? C88 C89 C90 120.2(3) . . ? C88 C89 H89 119.9 . . ? C90 C89 H89 119.9 . . ? C91 C90 C89 120.1(3) . . ? C91 C90 H90 120.0 . . ? C89 C90 H90 120.0 . . ? C90 C91 C92 120.4(3) . . ? C90 C91 H91 119.8 . . ? C92 C91 H91 119.8 . . ? C91 C92 C87 119.6(3) . . ? C91 C92 H92 120.2 . . ? C87 C92 H92 120.2 . . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.043 0.979 0.259 12 0 ' ' 2 0.198 0.538 0.202 154 41 ' ' 3 0.302 0.038 0.298 154 41 ' ' 4 0.457 0.479 0.241 12 0 ' ' 5 0.543 0.521 0.759 12 0 ' ' 6 0.698 0.962 0.702 154 41 ' ' 7 0.802 0.462 0.798 154 41 ' ' 8 0.957 0.021 0.741 12 0 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 24.77 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.255 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.052