# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Robert Mulvey' 'Nicholas D.R. Barnett' 'William Clegg' 'Alan R. Kennedy' 'Susan Weatherstone' _publ_contact_author_name 'Robert Mulvey' _publ_contact_author_address ; Department of Pure and Applied Chemistry University of Strathclyde Glasgow UK G1 1XL UNITED KINGDOM ; _publ_contact_author_email R.E.MULVEY@STRATH.AC.UK _publ_section_title ; Crystallographic characterisation of binary alkali metal alkoxide magnesium bis(alkyl) mixtures: differential binding of Na+ and K+ to a common dinuclear diorganomagnesiate ; data_rem36 _database_code_depnum_ccdc_archive 'CCDC 249271' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H86 Mg2 N4 Na2 O2' _chemical_formula_sum 'C36 H86 Mg2 N4 Na2 O2' _chemical_formula_weight 701.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.710(3) _cell_length_b 14.312(3) _cell_length_c 14.520(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.787(15) _cell_angle_gamma 90.00 _cell_volume 2382.1(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 32 _cell_measurement_theta_min 15.9 _cell_measurement_theta_max 19.1 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.978 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.847 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe-Siemens four-circle diffractometer' _diffrn_measurement_method '\w/\q scans with on-line profile fitting' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 5 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 4.3 _diffrn_reflns_number 3805 _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_sigmaI/netI 0.0572 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.38 _diffrn_reflns_theta_max 50.44 _reflns_number_total 2497 _reflns_number_gt 1472 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'local programs' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.1379P)^2^+1.6645P] 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 2497 _refine_ls_number_parameters 218 _refine_ls_number_restraints 46 _refine_ls_R_factor_all 0.1256 _refine_ls_R_factor_gt 0.0723 _refine_ls_wR_factor_ref 0.2511 _refine_ls_wR_factor_gt 0.2105 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.122 _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 Mg Mg 0.47535(18) 0.42981(14) 0.41917(12) 0.0743(7) Uani 1 1 d . . . Na Na 0.6068(2) 0.61671(18) 0.39280(15) 0.0875(9) Uani 1 1 d . . . N1 N 0.7927(7) 0.6680(7) 0.3405(6) 0.145(3) Uani 1 1 d U . . N2 N 0.5489(7) 0.7544(5) 0.2762(5) 0.124(2) Uani 1 1 d U . . C1 C 0.8388(14) 0.5904(11) 0.2935(12) 0.267(7) Uani 1 1 d U . . H1A H 0.8640 0.5413 0.3381 0.400 Uiso 1 1 calc R . . H1B H 0.9038 0.6117 0.2682 0.400 Uiso 1 1 calc R . . H1C H 0.7789 0.5672 0.2435 0.400 Uiso 1 1 calc R . . C2 C 0.8770(11) 0.7046(12) 0.4169(9) 0.260(8) Uani 1 1 d U . . H2A H 0.9001 0.6567 0.4632 0.390 Uiso 1 1 calc R . . H2B H 0.8437 0.7560 0.4447 0.390 Uiso 1 1 calc R . . H2C H 0.9440 0.7258 0.3942 0.390 Uiso 1 1 calc R . . C3 C 0.7587(12) 0.7417(10) 0.2725(9) 0.193(5) Uani 1 1 d U . . H3A H 0.8196 0.7887 0.2854 0.232 Uiso 1 1 calc R . . H3B H 0.7616 0.7154 0.2114 0.232 Uiso 1 1 calc R . . C4 C 0.6603(13) 0.7859(12) 0.2627(12) 0.264(8) Uani 1 1 d U . . H4A H 0.6458 0.8097 0.1988 0.317 Uiso 1 1 calc R . . H4B H 0.6776 0.8402 0.3031 0.317 Uiso 1 1 calc R . . C5 C 0.4792(16) 0.7256(8) 0.1887(8) 0.259(8) Uani 1 1 d U . . H5A H 0.5176 0.6757 0.1629 0.389 Uiso 1 1 calc R . . H5B H 0.4681 0.7774 0.1457 0.389 Uiso 1 1 calc R . . H5C H 0.4047 0.7043 0.1983 0.389 Uiso 1 1 calc R . . C6 C 0.4867(16) 0.8284(9) 0.3104(9) 0.239(7) Uani 1 1 d U . . H6A H 0.4116 0.8061 0.3173 0.358 Uiso 1 1 calc R . . H6B H 0.4768 0.8794 0.2665 0.358 Uiso 1 1 calc R . . H6C H 0.5299 0.8492 0.3703 0.358 Uiso 1 1 calc R . . O1 O 0.6146(3) 0.4845(3) 0.5100(3) 0.0785(12) Uani 1 1 d U . . C7 C 0.7226(6) 0.4396(5) 0.5458(4) 0.0891(19) Uani 1 1 d U . . C8 C 0.7056(8) 0.3628(6) 0.6140(6) 0.132(3) Uani 1 1 d U . . H8A H 0.6773 0.3895 0.6657 0.198 Uiso 1 1 calc R . . H8B H 0.7787 0.3321 0.6372 0.198 Uiso 1 1 calc R . . H8C H 0.6499 0.3182 0.5822 0.198 Uiso 1 1 calc R . . C9 C 0.7681(8) 0.3966(6) 0.4646(5) 0.133(3) Uani 1 1 d U . . H9A H 0.7805 0.4450 0.4218 0.199 Uiso 1 1 calc R . . H9B H 0.7122 0.3526 0.4322 0.199 Uiso 1 1 calc R . . H9C H 0.8405 0.3651 0.4885 0.199 Uiso 1 1 calc R . . C10 C 0.8098(6) 0.5106(6) 0.5958(6) 0.133(3) Uani 1 1 d U . . H10A H 0.8209 0.5586 0.5523 0.200 Uiso 1 1 calc R . . H10B H 0.8829 0.4802 0.6199 0.200 Uiso 1 1 calc R . . H10C H 0.7808 0.5380 0.6469 0.200 Uiso 1 1 calc R . . C11 C 0.4939(6) 0.4689(5) 0.2772(4) 0.093(2) Uani 1 1 d U . . H11A H 0.4903 0.5365 0.2720 0.111 Uiso 1 1 calc R . . H11B H 0.5706 0.4497 0.2689 0.111 Uiso 1 1 calc R . . C12 C 0.4051(7) 0.4285(6) 0.1991(4) 0.113(3) Uani 1 1 d U . . H12A H 0.3293 0.4520 0.2051 0.136 Uiso 1 1 calc R . . H12B H 0.4042 0.3614 0.2082 0.136 Uiso 1 1 calc R . . C13 C 0.4190(8) 0.4466(7) 0.0991(4) 0.131(3) Uani 1 1 d U . . H13A H 0.4187 0.5136 0.0891 0.157 Uiso 1 1 calc R . . H13B H 0.4948 0.4235 0.0925 0.157 Uiso 1 1 calc R . . C14 C 0.3295(10) 0.4043(8) 0.0244(6) 0.194(5) Uani 1 1 d U . . H14A H 0.3458 0.4196 -0.0360 0.290 Uiso 1 1 calc R . . H14B H 0.2541 0.4281 0.0285 0.290 Uiso 1 1 calc R . . H14C H 0.3303 0.3377 0.0321 0.290 Uiso 1 1 calc R . . C15 C 0.4207(8) 0.2852(5) 0.4415(5) 0.120(3) Uani 1 1 d DU . . H15A H 0.4381 0.2727 0.5086 0.144 Uiso 0.706(15) 1 calc PR A 1 H15B H 0.3368 0.2813 0.4203 0.144 Uiso 0.706(15) 1 calc PR A 1 H15C H 0.4474 0.2736 0.5090 0.144 Uiso 0.294(15) 1 calc PR A 2 C16 C 0.4735(12) 0.2127(6) 0.3952(8) 0.195(5) Uani 1 1 d DU A . H16A H 0.5540 0.2031 0.4268 0.235 Uiso 1 1 calc R . . H16B H 0.4720 0.2296 0.3303 0.235 Uiso 1 1 calc R . . C17 C 0.4006(18) 0.1222(8) 0.4001(10) 0.300(12) Uani 1 1 d DU . . H17A H 0.3941 0.1111 0.4647 0.360 Uiso 0.706(15) 1 calc PR A 1 H17B H 0.3225 0.1309 0.3629 0.360 Uiso 0.706(15) 1 calc PR A 1 H17C H 0.4337 0.0715 0.3711 0.450 Uiso 0.294(15) 1 calc PR A 2 H17D H 0.3216 0.1324 0.3674 0.450 Uiso 0.294(15) 1 calc PR A 2 H17E H 0.4015 0.1072 0.4646 0.450 Uiso 0.294(15) 1 calc PR A 2 C18A C 0.449(2) 0.0486(11) 0.3683(14) 0.271(12) Uani 0.706(15) 1 d PDU A 1 H18A H 0.4016 -0.0055 0.3707 0.407 Uiso 0.706(15) 1 calc PR A 1 H18B H 0.5254 0.0384 0.4066 0.407 Uiso 0.706(15) 1 calc PR A 1 H18C H 0.4564 0.0597 0.3044 0.407 Uiso 0.706(15) 1 calc PR A 1 C18B C 0.2947(15) 0.2526(18) 0.419(3) 0.23(2) Uani 0.294(15) 1 d PDU A 2 H18D H 0.2471 0.2956 0.4449 0.347 Uiso 0.294(15) 1 calc PR A 2 H18E H 0.2893 0.1916 0.4449 0.347 Uiso 0.294(15) 1 calc PR A 2 H18F H 0.2682 0.2499 0.3516 0.347 Uiso 0.294(15) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg 0.0968(15) 0.0753(14) 0.0494(11) -0.0005(10) 0.0119(10) -0.0039(11) Na 0.1064(19) 0.0923(18) 0.0647(15) 0.0127(12) 0.0197(13) -0.0078(15) N1 0.134(6) 0.187(8) 0.117(5) 0.047(5) 0.030(4) -0.021(5) N2 0.161(6) 0.120(6) 0.093(4) 0.037(4) 0.033(4) 0.006(5) C1 0.284(16) 0.288(14) 0.296(16) 0.072(10) 0.219(14) 0.071(12) C2 0.173(11) 0.38(2) 0.197(11) 0.107(10) -0.033(8) -0.149(12) C3 0.164(8) 0.248(12) 0.172(9) 0.111(9) 0.045(8) -0.019(8) C4 0.188(10) 0.274(17) 0.339(18) 0.228(15) 0.072(10) 0.006(8) C5 0.44(2) 0.145(10) 0.135(8) 0.059(6) -0.087(11) -0.043(11) C6 0.405(18) 0.169(11) 0.169(9) 0.091(7) 0.120(11) 0.135(12) O1 0.084(3) 0.088(3) 0.060(2) -0.002(2) 0.0079(19) 0.005(2) C7 0.091(5) 0.105(5) 0.066(4) -0.003(3) 0.005(3) 0.014(4) C8 0.147(7) 0.144(7) 0.097(5) 0.033(5) 0.010(5) 0.039(5) C9 0.133(7) 0.170(8) 0.094(5) -0.022(5) 0.021(4) 0.044(6) C10 0.099(5) 0.158(7) 0.128(6) -0.039(6) -0.011(5) 0.003(5) C11 0.120(5) 0.102(5) 0.056(3) 0.000(3) 0.018(3) -0.011(4) C12 0.142(6) 0.138(7) 0.055(4) -0.006(4) 0.011(4) -0.018(5) C13 0.175(8) 0.155(8) 0.055(4) -0.012(4) 0.009(4) 0.004(6) C14 0.244(13) 0.245(13) 0.077(5) -0.032(7) -0.003(6) -0.060(10) C15 0.189(8) 0.100(5) 0.069(4) 0.001(4) 0.020(5) -0.035(6) C16 0.355(16) 0.081(6) 0.149(9) -0.026(6) 0.049(10) -0.007(8) C17 0.62(4) 0.086(7) 0.179(12) -0.020(8) 0.036(16) -0.078(13) C18A 0.45(3) 0.131(11) 0.193(19) -0.002(14) -0.02(2) -0.034(18) C18B 0.190(14) 0.048(17) 0.38(6) 0.00(2) -0.13(3) -0.024(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 Mg O1 2.033(4) . ? Mg O1 2.028(4) 3_666 ? Mg C11 2.190(6) . ? Mg C15 2.209(8) . ? Na N1 2.556(8) . ? Na N2 2.596(7) . ? Na O1 2.533(5) . ? Na C11 2.852(7) . ? Na C15 2.860(8) 3_666 ? N1 C1 1.463(15) . ? N1 C2 1.425(13) . ? N1 C3 1.444(12) . ? N2 C4 1.431(14) . ? N2 C5 1.424(12) . ? N2 C6 1.431(12) . ? C3 C4 1.297(16) . ? O1 Mg 2.028(4) 3_666 ? O1 C7 1.420(7) . ? C7 C8 1.520(10) . ? C7 C9 1.520(9) . ? C7 C10 1.516(10) . ? C11 C12 1.490(9) . ? C12 C13 1.516(9) . ? C13 C14 1.475(11) . ? C15 Na 2.860(8) 3_666 ? C15 C16 1.443(10) . ? C15 C18B 1.518(16) . ? C16 C17 1.561(14) . ? C17 C18A 1.326(17) . ? 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 O1 82.47(19) . 3_666 ? O1 Mg C11 106.9(2) . . ? O1 Mg C11 119.0(2) 3_666 . ? O1 Mg C15 118.9(3) . . ? O1 Mg C15 107.2(3) 3_666 . ? C11 Mg C15 117.7(3) . . ? N1 Na N2 73.3(3) . . ? N1 Na O1 119.9(2) . . ? N1 Na C11 111.0(3) . . ? N1 Na C15 111.0(3) . 3_666 ? N2 Na O1 166.8(2) . . ? N2 Na C11 98.7(2) . . ? N2 Na C15 96.7(2) . 3_666 ? O1 Na C11 77.90(17) . . ? O1 Na C15 78.23(18) . 3_666 ? C11 Na C15 137.8(2) . 3_666 ? Na N1 C1 109.7(7) . . ? Na N1 C2 111.8(7) . . ? Na N1 C3 106.3(7) . . ? C1 N1 C2 112.3(12) . . ? C1 N1 C3 108.2(10) . . ? C2 N1 C3 108.3(10) . . ? Na N2 C4 101.8(6) . . ? Na N2 C5 112.9(6) . . ? Na N2 C6 114.8(5) . . ? C4 N2 C5 110.0(11) . . ? C4 N2 C6 110.9(11) . . ? C5 N2 C6 106.5(11) . . ? N1 C3 C4 123.1(11) . . ? N2 C4 C3 130.2(13) . . ? Mg O1 Mg 97.53(18) . 3_666 ? Mg O1 Na 86.45(16) . . ? Mg O1 Na 86.46(16) 3_666 . ? Mg O1 C7 126.9(4) . . ? Mg O1 C7 127.2(3) 3_666 . ? Na O1 C7 119.4(4) . . ? O1 C7 C8 109.9(6) . . ? O1 C7 C9 109.1(5) . . ? O1 C7 C10 109.5(6) . . ? C8 C7 C9 109.0(7) . . ? C8 C7 C10 109.8(6) . . ? C9 C7 C10 109.5(6) . . ? Mg C11 Na 76.03(19) . . ? Mg C11 C12 115.4(5) . . ? Na C11 C12 154.6(6) . . ? C11 C12 C13 117.9(7) . . ? C12 C13 C14 115.7(8) . . ? Mg C15 Na 75.5(2) . 3_666 ? Mg C15 C16 116.2(6) . . ? Mg C15 C18B 123.6(12) . . ? Na C15 C16 151.4(7) 3_666 . ? Na C15 C18B 93.6(15) 3_666 . ? C16 C15 C18B 99.6(11) . . ? C15 C16 C17 106.6(10) . . ? C16 C17 C18A 111.4(16) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 50.44 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.349 _refine_diff_density_min -0.273 _refine_diff_density_rms 0.047 data_grem156 _database_code_depnum_ccdc_archive 'CCDC 249272' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H86 K2 Mg2 N4 O2' _chemical_formula_weight 733.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source K K 0.2009 0.2494 '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' O O 0.0106 0.0060 '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' 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' _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 11.4984(6) _cell_length_b 14.7210(11) _cell_length_c 14.4940(10) _cell_angle_alpha 90.00 _cell_angle_beta 103.391(4) _cell_angle_gamma 90.00 _cell_volume 2386.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4224 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 25.03 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.021 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 0.255 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22825 _diffrn_reflns_av_R_equivalents 0.088 _diffrn_reflns_av_sigmaI/netI 0.1023 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 24.98 _reflns_number_total 4156 _reflns_number_gt 2212 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Denzo & Collect' _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^)+(0.0700P)^2^+3.2000P] 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 4156 _refine_ls_number_parameters 221 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1612 _refine_ls_R_factor_gt 0.0762 _refine_ls_wR_factor_ref 0.1964 _refine_ls_wR_factor_gt 0.1597 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group K1 K 0.89826(10) 0.63267(7) 0.10653(7) 0.0535(4) Uani 1 1 d . . . Mg1 Mg 1.03169(13) 0.43785(10) 0.08909(9) 0.0395(4) Uani 1 1 d . . . O1 O 0.8927(2) 0.4699(2) -0.01839(19) 0.0511(9) Uani 1 1 d . . . N1 N 0.6937(3) 0.6858(3) 0.1706(3) 0.0587(11) Uani 1 1 d . . . N2 N 0.9267(4) 0.7927(3) 0.2183(3) 0.0648(12) Uani 1 1 d . . . C1 C 0.6104(5) 0.7150(5) 0.0847(4) 0.0841(19) Uani 1 1 d . . . H1A H 0.5354 0.7342 0.0999 0.126 Uiso 1 1 calc R . . H1B H 0.5947 0.6646 0.0394 0.126 Uiso 1 1 calc R . . H1C H 0.6448 0.7661 0.0567 0.126 Uiso 1 1 calc R . . C2 C 0.6418(6) 0.6100(5) 0.2141(5) 0.104(2) Uani 1 1 d . . . H2A H 0.6992 0.5898 0.2714 0.155 Uiso 1 1 calc R . . H2B H 0.6236 0.5595 0.1690 0.155 Uiso 1 1 calc R . . H2C H 0.5682 0.6303 0.2309 0.155 Uiso 1 1 calc R . . C3 C 0.7219(5) 0.7608(4) 0.2389(4) 0.0673(16) Uani 1 1 d . . . H3A H 0.7555 0.7350 0.3026 0.081 Uiso 1 1 calc R . . H3B H 0.6465 0.7922 0.2414 0.081 Uiso 1 1 calc R . . C4 C 0.8066(5) 0.8286(4) 0.2179(4) 0.0688(16) Uani 1 1 d . . . H4A H 0.8151 0.8781 0.2652 0.083 Uiso 1 1 calc R . . H4B H 0.7723 0.8553 0.1548 0.083 Uiso 1 1 calc R . . C5 C 0.9949(6) 0.8637(5) 0.1843(4) 0.100(2) Uani 1 1 d . . . H5A H 1.0064 0.9151 0.2284 0.150 Uiso 1 1 calc R . . H5B H 0.9512 0.8841 0.1214 0.150 Uiso 1 1 calc R . . H5C H 1.0730 0.8396 0.1801 0.150 Uiso 1 1 calc R . . C6 C 0.9897(5) 0.7638(5) 0.3117(4) 0.090(2) Uani 1 1 d . . . H6A H 0.9930 0.8140 0.3566 0.135 Uiso 1 1 calc R . . H6B H 1.0712 0.7455 0.3100 0.135 Uiso 1 1 calc R . . H6C H 0.9478 0.7122 0.3318 0.135 Uiso 1 1 calc R . . C7 C 0.7800(4) 0.4271(4) -0.0498(3) 0.0574(14) Uani 1 1 d . . . C8 C 0.7375(5) 0.3934(5) 0.0355(4) 0.098(2) Uani 1 1 d . . . H8A H 0.7956 0.3501 0.0712 0.147 Uiso 1 1 calc R . . H8B H 0.6598 0.3634 0.0143 0.147 Uiso 1 1 calc R . . H8C H 0.7295 0.4449 0.0764 0.147 Uiso 1 1 calc R . . C9 C 0.7898(5) 0.3473(4) -0.1140(4) 0.084(2) Uani 1 1 d . . . H9A H 0.8217 0.3684 -0.1674 0.126 Uiso 1 1 calc R . . H9B H 0.7105 0.3206 -0.1381 0.126 Uiso 1 1 calc R . . H9C H 0.8435 0.3015 -0.0780 0.126 Uiso 1 1 calc R . . C10 C 0.6917(5) 0.4949(5) -0.1058(4) 0.090(2) Uani 1 1 d . . . H10A H 0.6823 0.5459 -0.0647 0.136 Uiso 1 1 calc R . . H10B H 0.6142 0.4652 -0.1292 0.136 Uiso 1 1 calc R . . H10C H 0.7216 0.5174 -0.1596 0.136 Uiso 1 1 calc R . . C11 C 1.0129(5) 0.4809(4) 0.2301(3) 0.0430(12) Uani 1 1 d . . . C12 C 1.0892(4) 0.4248(3) 0.3104(3) 0.0495(12) Uani 1 1 d . . . H12A H 1.0675 0.3600 0.2988 0.059 Uiso 1 1 calc R . . H12B H 1.1740 0.4313 0.3076 0.059 Uiso 1 1 calc R . . C13 C 1.0784(5) 0.4490(4) 0.4106(3) 0.0648(15) Uani 1 1 d . . . H13A H 0.9951 0.4379 0.4152 0.078 Uiso 1 1 calc R . . H13B H 1.0947 0.5147 0.4211 0.078 Uiso 1 1 calc R . . C14 C 1.1625(6) 0.3960(5) 0.4896(4) 0.0879(19) Uani 1 1 d . . . H14A H 1.1480 0.3307 0.4796 0.132 Uiso 1 1 calc R . . H14B H 1.1477 0.4135 0.5511 0.132 Uiso 1 1 calc R . . H14C H 1.2456 0.4097 0.4886 0.132 Uiso 1 1 calc R . . C15A C 1.0575(11) 0.2873(9) 0.0723(8) 0.063(3) Uiso 0.50 1 d P . 1 H15A H 1.0005 0.2547 0.1023 0.075 Uiso 0.50 1 calc PR . 1 H15B H 1.0360 0.2727 0.0038 0.075 Uiso 0.50 1 calc PR . 1 C16A C 1.1703(11) 0.2540(10) 0.1098(9) 0.082(4) Uiso 0.50 1 d P . 1 H16A H 1.2006 0.2764 0.1753 0.098 Uiso 0.50 1 calc PR . 1 H16B H 1.2262 0.2732 0.0709 0.098 Uiso 0.50 1 calc PR . 1 C17A C 1.1569(15) 0.1377(11) 0.1090(11) 0.092(5) Uiso 0.50 1 d P A 1 H17A H 1.1905 0.1230 0.0537 0.110 Uiso 0.50 1 calc PR A 1 H17B H 1.2219 0.1223 0.1645 0.110 Uiso 0.50 1 calc PR A 1 C15B C 1.1411(12) 0.3167(7) 0.0942(7) 0.060(3) Uani 0.50 1 d P . 2 C16B C 1.0682(12) 0.2202(10) 0.0937(9) 0.083(4) Uiso 0.50 1 d P A 2 C17B C 1.1985(15) 0.1414(12) 0.0863(12) 0.103(5) Uiso 0.50 1 d P A 2 C18A C 1.0908(9) 0.0715(7) 0.1082(7) 0.179(4) Uiso 1 1 d . . . H18A H 1.1461 0.0218 0.1038 0.269 Uiso 1 1 d R A . H18B H 1.0259 0.0724 0.0508 0.269 Uiso 1 1 d R . . H18C H 1.0574 0.0623 0.1638 0.269 Uiso 1 1 d R . . H11A H 0.936(4) 0.475(3) 0.238(3) 0.032(11) Uiso 1 1 d . . . H11B H 1.035(3) 0.541(3) 0.248(3) 0.032(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 K1 0.0697(8) 0.0509(7) 0.0387(6) -0.0086(5) 0.0103(5) 0.0127(6) Mg1 0.0516(9) 0.0388(9) 0.0282(8) 0.0050(6) 0.0096(6) 0.0043(7) O1 0.0428(18) 0.077(2) 0.0288(16) 0.0091(16) -0.0015(13) -0.0234(17) N1 0.050(2) 0.069(3) 0.052(3) -0.023(2) 0.002(2) -0.005(2) N2 0.065(3) 0.077(3) 0.057(3) -0.028(2) 0.024(2) -0.018(3) C1 0.066(4) 0.119(5) 0.060(4) -0.029(4) -0.001(3) 0.014(4) C2 0.102(5) 0.112(6) 0.100(5) -0.021(4) 0.031(4) -0.044(4) C3 0.058(3) 0.088(4) 0.055(3) -0.024(3) 0.012(3) -0.001(3) C4 0.085(4) 0.064(4) 0.060(3) -0.020(3) 0.023(3) 0.002(3) C5 0.121(5) 0.108(6) 0.082(4) -0.042(4) 0.049(4) -0.057(5) C6 0.078(4) 0.101(5) 0.082(5) -0.021(4) 0.002(4) -0.006(4) C7 0.052(3) 0.089(4) 0.031(3) -0.006(3) 0.007(2) -0.028(3) C8 0.100(5) 0.150(6) 0.051(3) -0.016(4) 0.030(3) -0.078(5) C9 0.066(4) 0.122(6) 0.065(4) -0.028(4) 0.016(3) -0.037(4) C10 0.045(3) 0.127(6) 0.088(4) -0.003(4) -0.009(3) -0.017(4) C11 0.053(3) 0.044(3) 0.032(3) 0.000(2) 0.010(2) -0.008(3) C12 0.057(3) 0.061(3) 0.030(2) 0.006(2) 0.008(2) -0.005(3) C13 0.091(4) 0.066(4) 0.032(3) 0.005(3) 0.004(3) -0.003(3) C14 0.104(5) 0.106(5) 0.045(3) 0.020(3) 0.000(3) -0.002(4) C15B 0.094(9) 0.036(6) 0.056(7) 0.017(5) 0.027(6) 0.027(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 N1 2.831(4) . ? K1 N2 2.835(4) . ? K1 C15B 2.934(10) 3_765 ? K1 C11 2.974(5) . ? K1 O1 2.995(3) . ? K1 C15A 2.996(12) 3_765 ? K1 Mg1 3.2898(16) 3_765 ? K1 Mg1 3.2898(17) . ? K1 O1 3.333(3) 3_765 ? K1 C16A 3.477(14) 3_765 ? K1 H11A 2.97(4) . ? K1 H11B 2.65(4) . ? Mg1 O1 2.012(3) . ? Mg1 O1 2.016(3) 3_765 ? Mg1 C15B 2.174(11) . ? Mg1 C11 2.197(5) . ? Mg1 C15A 2.257(13) . ? Mg1 Mg1 3.111(3) 3_765 ? Mg1 K1 3.2898(16) 3_765 ? O1 C7 1.418(5) . ? O1 Mg1 2.016(3) 3_765 ? O1 K1 3.333(3) 3_765 ? N1 C1 1.449(6) . ? N1 C3 1.468(6) . ? N1 C2 1.474(7) . ? N2 C6 1.444(7) . ? N2 C5 1.459(7) . ? N2 C4 1.477(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.475(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? 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 1.515(6) . ? C7 C10 1.518(8) . ? C7 C9 1.518(7) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? 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 1.528(6) . ? C11 H11A 0.92(4) . ? C11 H11B 0.95(4) . ? C12 C13 1.528(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.530(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15A C16A 1.375(16) . ? C15A K1 2.996(12) 3_765 ? C15A H15A 0.9900 . ? C15A H15B 0.9900 . ? C16A C17A 1.72(2) . ? C16A K1 3.477(14) 3_765 ? C16A H16A 0.9900 . ? C16A H16B 0.9900 . ? C17A C18A 1.235(16) . ? C17A H17A 0.9900 . ? C17A H17B 0.9900 . ? C15B C16B 1.649(18) . ? C15B K1 2.934(10) 3_765 ? C16B C17B 1.92(2) . ? C17B C18A 1.70(2) . ? C18A H18A 0.9800 . ? C18A H18B 0.9800 . ? C18A H18C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 K1 N2 65.03(12) . . ? N1 K1 C15B 107.8(3) . 3_765 ? N2 K1 C15B 109.0(2) . 3_765 ? N1 K1 C11 107.23(14) . . ? N2 K1 C11 107.71(14) . . ? C15B K1 C11 137.1(2) 3_765 . ? N1 K1 O1 121.08(10) . . ? N2 K1 O1 173.62(11) . . ? C15B K1 O1 68.1(2) 3_765 . ? C11 K1 O1 72.97(11) . . ? N1 K1 C15A 119.7(2) . 3_765 ? N2 K1 C15A 98.5(3) . 3_765 ? C15B K1 C15A 20.1(3) 3_765 3_765 ? C11 K1 C15A 132.5(2) . 3_765 ? O1 K1 C15A 77.0(2) . 3_765 ? N1 K1 Mg1 139.25(9) . 3_765 ? N2 K1 Mg1 137.37(10) . 3_765 ? C15B K1 Mg1 40.4(2) 3_765 3_765 ? C11 K1 Mg1 96.83(9) . 3_765 ? O1 K1 Mg1 37.04(6) . 3_765 ? C15A K1 Mg1 41.7(2) 3_765 3_765 ? N1 K1 Mg1 134.71(10) . . ? N2 K1 Mg1 140.74(11) . . ? C15B K1 Mg1 96.5(2) 3_765 . ? C11 K1 Mg1 40.67(9) . . ? O1 K1 Mg1 36.97(6) . . ? C15A K1 Mg1 95.8(2) 3_765 . ? Mg1 K1 Mg1 56.43(4) 3_765 . ? N1 K1 O1 168.03(10) . 3_765 ? N2 K1 O1 126.68(10) . 3_765 ? C15B K1 O1 72.2(2) 3_765 3_765 ? C11 K1 O1 68.41(10) . 3_765 ? O1 K1 O1 47.33(9) . 3_765 ? C15A K1 O1 64.2(2) 3_765 3_765 ? Mg1 K1 O1 35.37(5) 3_765 3_765 ? Mg1 K1 O1 35.43(6) . 3_765 ? N1 K1 C16A 97.5(2) . 3_765 ? N2 K1 C16A 95.1(2) . 3_765 ? C15B K1 C16A 14.9(3) 3_765 3_765 ? C11 K1 C16A 151.6(2) . 3_765 ? O1 K1 C16A 82.5(2) . 3_765 ? C15A K1 C16A 23.0(3) 3_765 3_765 ? Mg1 K1 C16A 54.8(2) 3_765 3_765 ? Mg1 K1 C16A 111.2(2) . 3_765 ? O1 K1 C16A 84.5(2) 3_765 3_765 ? N1 K1 H11A 90.9(8) . . ? N2 K1 H11A 107.7(7) . . ? C15B K1 H11A 143.1(7) 3_765 . ? C11 K1 H11A 17.8(7) . . ? O1 K1 H11A 75.0(7) . . ? C15A K1 H11A 146.3(8) 3_765 . ? Mg1 K1 H11A 106.0(7) 3_765 . ? Mg1 K1 H11A 50.6(7) . . ? O1 K1 H11A 83.1(7) 3_765 . ? C16A K1 H11A 157.2(7) 3_765 . ? N1 K1 H11B 106.0(7) . . ? N2 K1 H11B 90.5(9) . . ? C15B K1 H11B 145.7(8) 3_765 . ? C11 K1 H11B 18.2(9) . . ? O1 K1 H11B 89.4(9) . . ? C15A K1 H11B 133.0(8) 3_765 . ? Mg1 K1 H11B 106.8(8) 3_765 . ? Mg1 K1 H11B 54.1(9) . . ? O1 K1 H11B 73.5(8) 3_765 . ? C16A K1 H11B 156.0(8) 3_765 . ? H11A K1 H11B 29.9(10) . . ? O1 Mg1 O1 78.87(13) . 3_765 ? O1 Mg1 C15B 124.6(3) . . ? O1 Mg1 C15B 104.8(3) 3_765 . ? O1 Mg1 C11 114.90(17) . . ? O1 Mg1 C11 115.18(18) 3_765 . ? C15B Mg1 C11 112.7(3) . . ? O1 Mg1 C15A 104.3(3) . . ? O1 Mg1 C15A 121.6(3) 3_765 . ? C15B Mg1 C15A 27.0(3) . . ? C11 Mg1 C15A 115.3(3) . . ? O1 Mg1 Mg1 39.48(8) . 3_765 ? O1 Mg1 Mg1 39.40(9) 3_765 3_765 ? C15B Mg1 Mg1 122.2(3) . 3_765 ? C11 Mg1 Mg1 123.23(15) . 3_765 ? C15A Mg1 Mg1 120.0(3) . 3_765 ? O1 Mg1 K1 73.48(10) . 3_765 ? O1 Mg1 K1 63.52(10) 3_765 3_765 ? C15B Mg1 K1 61.0(3) . 3_765 ? C11 Mg1 K1 171.45(15) . 3_765 ? C15A Mg1 K1 62.1(3) . 3_765 ? Mg1 Mg1 K1 61.79(5) 3_765 3_765 ? O1 Mg1 K1 63.54(10) . . ? O1 Mg1 K1 73.45(10) 3_765 . ? C15B Mg1 K1 171.5(4) . . ? C11 Mg1 K1 61.92(13) . . ? C15A Mg1 K1 160.0(3) . . ? Mg1 Mg1 K1 61.78(5) 3_765 . ? K1 Mg1 K1 123.57(4) 3_765 . ? C7 O1 Mg1 130.3(3) . . ? C7 O1 Mg1 127.3(3) . 3_765 ? Mg1 O1 Mg1 101.13(13) . 3_765 ? C7 O1 K1 116.1(3) . . ? Mg1 O1 K1 79.49(10) . . ? Mg1 O1 K1 79.44(11) 3_765 . ? C7 O1 K1 111.2(3) . 3_765 ? Mg1 O1 K1 71.15(10) . 3_765 ? Mg1 O1 K1 71.12(9) 3_765 3_765 ? K1 O1 K1 132.67(9) . 3_765 ? C1 N1 C3 110.8(4) . . ? C1 N1 C2 109.9(5) . . ? C3 N1 C2 109.2(4) . . ? C1 N1 K1 103.5(3) . . ? C3 N1 K1 111.0(3) . . ? C2 N1 K1 112.4(4) . . ? C6 N2 C5 109.6(5) . . ? C6 N2 C4 112.0(4) . . ? C5 N2 C4 108.5(5) . . ? C6 N2 K1 104.9(4) . . ? C5 N2 K1 113.7(3) . . ? C4 N2 K1 108.1(3) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C4 115.0(4) . . ? N1 C3 H3A 108.5 . . ? C4 C3 H3A 108.5 . . ? N1 C3 H3B 108.5 . . ? C4 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? C3 C4 N2 114.8(5) . . ? C3 C4 H4A 108.6 . . ? N2 C4 H4A 108.6 . . ? C3 C4 H4B 108.6 . . ? N2 C4 H4B 108.6 . . ? H4A C4 H4B 107.5 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O1 C7 C8 109.1(4) . . ? O1 C7 C10 109.1(4) . . ? C8 C7 C10 110.4(5) . . ? O1 C7 C9 110.4(4) . . ? C8 C7 C9 109.3(5) . . ? C10 C7 C9 108.5(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 Mg1 113.0(3) . . ? C12 C11 K1 164.0(4) . . ? Mg1 C11 K1 77.41(13) . . ? C12 C11 H11A 105(2) . . ? Mg1 C11 H11A 113(2) . . ? K1 C11 H11A 81(2) . . ? C12 C11 H11B 103(2) . . ? Mg1 C11 H11B 117(2) . . ? K1 C11 H11B 61(2) . . ? H11A C11 H11B 105(3) . . ? C13 C12 C11 116.1(4) . . ? C13 C12 H12A 108.3 . . ? C11 C12 H12A 108.3 . . ? C13 C12 H12B 108.3 . . ? C11 C12 H12B 108.3 . . ? H12A C12 H12B 107.4 . . ? C12 C13 C14 114.6(5) . . ? C12 C13 H13A 108.6 . . ? C14 C13 H13A 108.6 . . ? C12 C13 H13B 108.6 . . ? C14 C13 H13B 108.6 . . ? H13A C13 H13B 107.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16A C15A Mg1 116.3(10) . . ? C16A C15A K1 98.5(8) . 3_765 ? Mg1 C15A K1 76.1(4) . 3_765 ? C16A C15A H15A 108.2 . . ? Mg1 C15A H15A 108.2 . . ? K1 C15A H15A 146.4 3_765 . ? C16A C15A H15B 108.2 . . ? Mg1 C15A H15B 108.2 . . ? K1 C15A H15B 43.1 3_765 . ? H15A C15A H15B 107.4 . . ? C15A C16A C17A 106.1(11) . . ? C15A C16A K1 58.4(7) . 3_765 ? C17A C16A K1 118.1(8) . 3_765 ? C15A C16A H16A 110.5 . . ? C17A C16A H16A 110.5 . . ? K1 C16A H16A 131.4 3_765 . ? C15A C16A H16B 110.5 . . ? C17A C16A H16B 110.5 . . ? K1 C16A H16B 52.4 3_765 . ? H16A C16A H16B 108.7 . . ? C18A C17A C16A 147.2(15) . . ? C18A C17A H17A 100.0 . . ? C16A C17A H17A 100.0 . . ? C18A C17A H17B 100.0 . . ? C16A C17A H17B 100.0 . . ? H17A C17A H17B 104.2 . . ? C16B C15B Mg1 114.6(9) . . ? C16B C15B K1 104.6(7) . 3_765 ? Mg1 C15B K1 78.6(3) . 3_765 ? C15B C16B C17B 96.8(9) . . ? C18A C17B C16B 75.1(9) . . ? C17A C18A C17B 17.8(10) . . ? C17A C18A H18A 100.5 . . ? C17B C18A H18A 85.9 . . ? C17A C18A H18B 110.1 . . ? C17B C18A H18B 106.2 . . ? H18A C18A H18B 109.5 . . ? C17A C18A H18C 117.3 . . ? C17B C18A H18C 132.9 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 K1 Mg1 O1 83.84(15) . . . . ? N2 K1 Mg1 O1 -170.34(17) . . . . ? C15B K1 Mg1 O1 -39.2(3) 3_765 . . . ? C11 K1 Mg1 O1 142.99(19) . . . . ? C15A K1 Mg1 O1 -59.4(3) 3_765 . . . ? Mg1 K1 Mg1 O1 -44.65(9) 3_765 . . . ? O1 K1 Mg1 O1 -85.59(13) 3_765 . . . ? C16A K1 Mg1 O1 -41.7(2) 3_765 . . . ? N1 K1 Mg1 O1 169.42(15) . . . 3_765 ? N2 K1 Mg1 O1 -84.75(17) . . . 3_765 ? C15B K1 Mg1 O1 46.4(3) 3_765 . . 3_765 ? C11 K1 Mg1 O1 -131.42(19) . . . 3_765 ? O1 K1 Mg1 O1 85.59(13) . . . 3_765 ? C15A K1 Mg1 O1 26.2(3) 3_765 . . 3_765 ? Mg1 K1 Mg1 O1 40.94(9) 3_765 . . 3_765 ? C16A K1 Mg1 O1 43.9(2) 3_765 . . 3_765 ? N1 K1 Mg1 C15B -111.2(19) . . . . ? N2 K1 Mg1 C15B -5.4(19) . . . . ? C15B K1 Mg1 C15B 125.7(17) 3_765 . . . ? C11 K1 Mg1 C15B -52.1(19) . . . . ? O1 K1 Mg1 C15B 164.9(19) . . . . ? C15A K1 Mg1 C15B 105.5(18) 3_765 . . . ? Mg1 K1 Mg1 C15B 120.3(19) 3_765 . . . ? O1 K1 Mg1 C15B 79.3(19) 3_765 . . . ? C16A K1 Mg1 C15B 123.2(19) 3_765 . . . ? N1 K1 Mg1 C11 -59.2(2) . . . . ? N2 K1 Mg1 C11 46.7(2) . . . . ? C15B K1 Mg1 C11 177.8(3) 3_765 . . . ? O1 K1 Mg1 C11 -142.99(19) . . . . ? C15A K1 Mg1 C11 157.6(3) 3_765 . . . ? Mg1 K1 Mg1 C11 172.36(18) 3_765 . . . ? O1 K1 Mg1 C11 131.42(19) 3_765 . . . ? C16A K1 Mg1 C11 175.3(3) 3_765 . . . ? N1 K1 Mg1 C15A 27.9(9) . . . . ? N2 K1 Mg1 C15A 133.7(9) . . . . ? C15B K1 Mg1 C15A -95.1(9) 3_765 . . . ? C11 K1 Mg1 C15A 87.1(9) . . . . ? O1 K1 Mg1 C15A -55.9(9) . . . . ? C15A K1 Mg1 C15A -115.3(8) 3_765 . . . ? Mg1 K1 Mg1 C15A -100.6(9) 3_765 . . . ? O1 K1 Mg1 C15A -141.5(9) 3_765 . . . ? C16A K1 Mg1 C15A -97.7(9) 3_765 . . . ? N1 K1 Mg1 Mg1 128.49(13) . . . 3_765 ? N2 K1 Mg1 Mg1 -125.69(15) . . . 3_765 ? C15B K1 Mg1 Mg1 5.4(3) 3_765 . . 3_765 ? C11 K1 Mg1 Mg1 -172.36(18) . . . 3_765 ? O1 K1 Mg1 Mg1 44.65(9) . . . 3_765 ? C15A K1 Mg1 Mg1 -14.7(3) 3_765 . . 3_765 ? O1 K1 Mg1 Mg1 -40.94(9) 3_765 . . 3_765 ? C16A K1 Mg1 Mg1 2.9(2) 3_765 . . 3_765 ? N1 K1 Mg1 K1 128.49(13) . . . 3_765 ? N2 K1 Mg1 K1 -125.69(15) . . . 3_765 ? C15B K1 Mg1 K1 5.4(3) 3_765 . . 3_765 ? C11 K1 Mg1 K1 -172.36(18) . . . 3_765 ? O1 K1 Mg1 K1 44.65(9) . . . 3_765 ? C15A K1 Mg1 K1 -14.7(3) 3_765 . . 3_765 ? Mg1 K1 Mg1 K1 0.0 3_765 . . 3_765 ? O1 K1 Mg1 K1 -40.94(9) 3_765 . . 3_765 ? C16A K1 Mg1 K1 2.9(2) 3_765 . . 3_765 ? O1 Mg1 O1 C7 167.7(4) 3_765 . . . ? C15B Mg1 O1 C7 67.3(5) . . . . ? C11 Mg1 O1 C7 -79.6(4) . . . . ? C15A Mg1 O1 C7 47.6(5) . . . . ? Mg1 Mg1 O1 C7 167.7(4) 3_765 . . . ? K1 Mg1 O1 C7 102.3(4) 3_765 . . . ? K1 Mg1 O1 C7 -115.4(4) . . . . ? O1 Mg1 O1 Mg1 0.0 3_765 . . 3_765 ? C15B Mg1 O1 Mg1 -100.4(4) . . . 3_765 ? C11 Mg1 O1 Mg1 112.8(2) . . . 3_765 ? C15A Mg1 O1 Mg1 -120.1(3) . . . 3_765 ? K1 Mg1 O1 Mg1 -65.44(11) 3_765 . . 3_765 ? K1 Mg1 O1 Mg1 76.92(12) . . . 3_765 ? O1 Mg1 O1 K1 -76.92(12) 3_765 . . . ? C15B Mg1 O1 K1 -177.3(4) . . . . ? C11 Mg1 O1 K1 35.84(18) . . . . ? C15A Mg1 O1 K1 163.0(3) . . . . ? Mg1 Mg1 O1 K1 -76.92(12) 3_765 . . . ? K1 Mg1 O1 K1 -142.36(6) 3_765 . . . ? O1 Mg1 O1 K1 65.44(11) 3_765 . . 3_765 ? C15B Mg1 O1 K1 -35.0(4) . . . 3_765 ? C11 Mg1 O1 K1 178.19(17) . . . 3_765 ? C15A Mg1 O1 K1 -54.6(3) . . . 3_765 ? Mg1 Mg1 O1 K1 65.44(11) 3_765 . . 3_765 ? K1 Mg1 O1 K1 142.36(6) . . . 3_765 ? N1 K1 O1 C7 5.5(3) . . . . ? N2 K1 O1 C7 -157.2(11) . . . . ? C15B K1 O1 C7 -92.6(4) 3_765 . . . ? C11 K1 O1 C7 105.7(3) . . . . ? C15A K1 O1 C7 -111.5(4) 3_765 . . . ? Mg1 K1 O1 C7 -126.5(3) 3_765 . . . ? Mg1 K1 O1 C7 130.0(3) . . . . ? O1 K1 O1 C7 -178.2(4) 3_765 . . . ? C16A K1 O1 C7 -88.8(3) 3_765 . . . ? N1 K1 O1 Mg1 -124.42(13) . . . . ? N2 K1 O1 Mg1 72.9(11) . . . . ? C15B K1 O1 Mg1 137.4(3) 3_765 . . . ? C11 K1 O1 Mg1 -24.22(13) . . . . ? C15A K1 O1 Mg1 118.5(2) 3_765 . . . ? Mg1 K1 O1 Mg1 103.54(12) 3_765 . . . ? O1 K1 O1 Mg1 51.83(10) 3_765 . . . ? C16A K1 O1 Mg1 141.2(2) 3_765 . . . ? N1 K1 O1 Mg1 132.04(13) . . . 3_765 ? N2 K1 O1 Mg1 -30.7(11) . . . 3_765 ? C15B K1 O1 Mg1 33.9(3) 3_765 . . 3_765 ? C11 K1 O1 Mg1 -127.77(14) . . . 3_765 ? C15A K1 O1 Mg1 15.0(2) 3_765 . . 3_765 ? Mg1 K1 O1 Mg1 -103.54(12) . . . 3_765 ? O1 K1 O1 Mg1 -51.72(9) 3_765 . . 3_765 ? C16A K1 O1 Mg1 37.7(2) 3_765 . . 3_765 ? N1 K1 O1 K1 -176.24(14) . . . 3_765 ? N2 K1 O1 K1 21.0(11) . . . 3_765 ? C15B K1 O1 K1 85.6(3) 3_765 . . 3_765 ? C11 K1 O1 K1 -76.05(16) . . . 3_765 ? C15A K1 O1 K1 66.7(3) 3_765 . . 3_765 ? Mg1 K1 O1 K1 51.72(9) 3_765 . . 3_765 ? Mg1 K1 O1 K1 -51.83(10) . . . 3_765 ? O1 K1 O1 K1 0.0 3_765 . . 3_765 ? C16A K1 O1 K1 89.4(2) 3_765 . . 3_765 ? N2 K1 N1 C1 110.5(4) . . . . ? C15B K1 N1 C1 7.3(4) 3_765 . . . ? C11 K1 N1 C1 -147.5(3) . . . . ? O1 K1 N1 C1 -67.4(4) . . . . ? C15A K1 N1 C1 25.0(5) 3_765 . . . ? Mg1 K1 N1 C1 -24.1(4) 3_765 . . . ? Mg1 K1 N1 C1 -111.7(3) . . . . ? O1 K1 N1 C1 -80.8(6) 3_765 . . . ? C16A K1 N1 C1 18.4(4) 3_765 . . . ? N2 K1 N1 C3 -8.4(3) . . . . ? C15B K1 N1 C3 -111.6(4) 3_765 . . . ? C11 K1 N1 C3 93.5(4) . . . . ? O1 K1 N1 C3 173.7(3) . . . . ? C15A K1 N1 C3 -93.9(4) 3_765 . . . ? Mg1 K1 N1 C3 -143.1(3) 3_765 . . . ? Mg1 K1 N1 C3 129.4(3) . . . . ? O1 K1 N1 C3 160.3(4) 3_765 . . . ? C16A K1 N1 C3 -100.5(4) 3_765 . . . ? N2 K1 N1 C2 -131.0(4) . . . . ? C15B K1 N1 C2 125.8(4) 3_765 . . . ? C11 K1 N1 C2 -29.0(4) . . . . ? O1 K1 N1 C2 51.1(4) . . . . ? C15A K1 N1 C2 143.5(4) 3_765 . . . ? Mg1 K1 N1 C2 94.4(4) 3_765 . . . ? Mg1 K1 N1 C2 6.8(4) . . . . ? O1 K1 N1 C2 37.7(7) 3_765 . . . ? C16A K1 N1 C2 136.9(4) 3_765 . . . ? N1 K1 N2 C6 100.3(3) . . . . ? C15B K1 N2 C6 -158.4(4) 3_765 . . . ? C11 K1 N2 C6 -0.9(4) . . . . ? O1 K1 N2 C6 -96.0(11) . . . . ? C15A K1 N2 C6 -140.8(4) 3_765 . . . ? Mg1 K1 N2 C6 -123.0(3) 3_765 . . . ? Mg1 K1 N2 C6 -30.7(4) . . . . ? O1 K1 N2 C6 -76.8(3) 3_765 . . . ? C16A K1 N2 C6 -163.7(4) 3_765 . . . ? N1 K1 N2 C5 -139.9(5) . . . . ? C15B K1 N2 C5 -38.6(5) 3_765 . . . ? C11 K1 N2 C5 118.9(4) . . . . ? O1 K1 N2 C5 23.8(13) . . . . ? C15A K1 N2 C5 -21.0(5) 3_765 . . . ? Mg1 K1 N2 C5 -3.2(5) 3_765 . . . ? Mg1 K1 N2 C5 89.0(4) . . . . ? O1 K1 N2 C5 43.0(5) 3_765 . . . ? C16A K1 N2 C5 -44.0(5) 3_765 . . . ? N1 K1 N2 C4 -19.3(3) . . . . ? C15B K1 N2 C4 82.0(4) 3_765 . . . ? C11 K1 N2 C4 -120.5(3) . . . . ? O1 K1 N2 C4 144.4(10) . . . . ? C15A K1 N2 C4 99.6(4) 3_765 . . . ? Mg1 K1 N2 C4 117.4(3) 3_765 . . . ? Mg1 K1 N2 C4 -150.4(3) . . . . ? O1 K1 N2 C4 163.6(3) 3_765 . . . ? C16A K1 N2 C4 76.6(4) 3_765 . . . ? C1 N1 C3 C4 -76.9(6) . . . . ? C2 N1 C3 C4 161.9(5) . . . . ? K1 N1 C3 C4 37.5(5) . . . . ? N1 C3 C4 N2 -62.3(6) . . . . ? C6 N2 C4 C3 -66.3(6) . . . . ? C5 N2 C4 C3 172.5(4) . . . . ? K1 N2 C4 C3 48.8(5) . . . . ? Mg1 O1 C7 C8 37.4(6) . . . . ? Mg1 O1 C7 C8 -157.8(4) 3_765 . . . ? K1 O1 C7 C8 -61.1(5) . . . . ? K1 O1 C7 C8 120.3(4) 3_765 . . . ? Mg1 O1 C7 C10 158.2(3) . . . . ? Mg1 O1 C7 C10 -37.1(5) 3_765 . . . ? K1 O1 C7 C10 59.6(4) . . . . ? K1 O1 C7 C10 -119.0(4) 3_765 . . . ? Mg1 O1 C7 C9 -82.7(5) . . . . ? Mg1 O1 C7 C9 82.0(5) 3_765 . . . ? K1 O1 C7 C9 178.7(3) . . . . ? K1 O1 C7 C9 0.1(5) 3_765 . . . ? O1 Mg1 C11 C12 156.4(3) . . . . ? O1 Mg1 C11 C12 -114.6(3) 3_765 . . . ? C15B Mg1 C11 C12 5.6(6) . . . . ? C15A Mg1 C11 C12 35.0(5) . . . . ? Mg1 Mg1 C11 C12 -159.1(3) 3_765 . . . ? K1 Mg1 C11 C12 -35.4(13) 3_765 . . . ? K1 Mg1 C11 C12 -167.2(4) . . . . ? O1 Mg1 C11 K1 -36.45(17) . . . . ? O1 Mg1 C11 K1 52.59(17) 3_765 . . . ? C15B Mg1 C11 K1 172.8(4) . . . . ? C15A Mg1 C11 K1 -157.8(4) . . . . ? Mg1 Mg1 C11 K1 8.05(19) 3_765 . . . ? K1 Mg1 C11 K1 131.8(10) 3_765 . . . ? N1 K1 C11 C12 -87.5(12) . . . . ? N2 K1 C11 C12 -18.9(12) . . . . ? C15B K1 C11 C12 129.0(12) 3_765 . . . ? O1 K1 C11 C12 154.4(12) . . . . ? C15A K1 C11 C12 101.3(12) 3_765 . . . ? Mg1 K1 C11 C12 125.8(12) 3_765 . . . ? Mg1 K1 C11 C12 132.2(12) . . . . ? O1 K1 C11 C12 104.3(12) 3_765 . . . ? C16A K1 C11 C12 122.9(12) 3_765 . . . ? N1 K1 C11 Mg1 140.30(14) . . . . ? N2 K1 C11 Mg1 -151.10(14) . . . . ? C15B K1 C11 Mg1 -3.2(5) 3_765 . . . ? O1 K1 C11 Mg1 22.25(12) . . . . ? C15A K1 C11 Mg1 -30.9(4) 3_765 . . . ? Mg1 K1 C11 Mg1 -6.41(15) 3_765 . . . ? O1 K1 C11 Mg1 -27.87(11) 3_765 . . . ? C16A K1 C11 Mg1 -9.3(6) 3_765 . . . ? Mg1 C11 C12 C13 -178.4(3) . . . . ? K1 C11 C12 C13 53.3(13) . . . . ? C11 C12 C13 C14 -175.9(5) . . . . ? O1 Mg1 C15A C16A 155.0(9) . . . . ? O1 Mg1 C15A C16A 69.4(10) 3_765 . . . ? C15B Mg1 C15A C16A 12.6(9) . . . . ? C11 Mg1 C15A C16A -78.1(10) . . . . ? Mg1 Mg1 C15A C16A 115.5(9) 3_765 . . . ? K1 Mg1 C15A C16A 92.8(10) 3_765 . . . ? K1 Mg1 C15A C16A -155.1(7) . . . . ? O1 Mg1 C15A K1 62.2(2) . . . 3_765 ? O1 Mg1 C15A K1 -23.4(4) 3_765 . . 3_765 ? C15B Mg1 C15A K1 -80.2(9) . . . 3_765 ? C11 Mg1 C15A K1 -170.89(17) . . . 3_765 ? Mg1 Mg1 C15A K1 22.8(3) 3_765 . . 3_765 ? K1 Mg1 C15A K1 112.1(8) . . . 3_765 ? Mg1 C15A C16A C17A 167.9(8) . . . . ? K1 C15A C16A C17A -113.4(9) 3_765 . . . ? Mg1 C15A C16A K1 -78.7(7) . . . 3_765 ? C15A C16A C17A C18A -23(3) . . . . ? K1 C16A C17A C18A -86(3) 3_765 . . . ? O1 Mg1 C15B C16B -62.1(7) . . . . ? O1 Mg1 C15B C16B -148.7(7) 3_765 . . . ? C11 Mg1 C15B C16B 85.4(8) . . . . ? C15A Mg1 C15B C16B -16.1(9) . . . . ? Mg1 Mg1 C15B C16B -109.8(6) 3_765 . . . ? K1 Mg1 C15B C16B -101.0(8) 3_765 . . . ? K1 Mg1 C15B C16B 134.3(18) . . . . ? O1 Mg1 C15B K1 38.9(4) . . . 3_765 ? O1 Mg1 C15B K1 -47.6(3) 3_765 . . 3_765 ? C11 Mg1 C15B K1 -173.60(18) . . . 3_765 ? C15A Mg1 C15B K1 84.9(9) . . . 3_765 ? Mg1 Mg1 C15B K1 -8.7(4) 3_765 . . 3_765 ? K1 Mg1 C15B K1 -124.6(17) . . . 3_765 ? Mg1 C15B C16B C17B 174.7(7) . . . . ? K1 C15B C16B C17B 90.7(8) 3_765 . . . ? C15B C16B C17B C18A 170.1(9) . . . . ? C16A C17A C18A C17B 141(6) . . . . ? C16B C17B C18A C17A -37(4) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.598 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.057