Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Marc Hillmyer' 'Laurie E. Breyfogle' 'William Tolman' 'Charlotte K. Williams' 'Victor G. Young' _publ_contact_author_name 'Prof Marc Hillmyer' _publ_contact_author_address ; Department of Chemistry University of Minnesoa 207 Pleasant St. Minneapolis Minnesota MN 55455-0431 UNITED STATES OF AMERICA ; _publ_contact_author_email HILLMYER@CHEM.UMN.EDU _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Comparison of Structurally Analogous Zn2, Co2, and Mg2 Catalysts for the Polymerization of Cyclic Esters ; data_02080 _database_code_depnum_ccdc_archive 'CCDC 189527' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 02080 _chemical_formula_moiety 'C21 H40 Cl2 N4 O2 Zn2, C4 H8 O' _chemical_formula_sum 'C25 H48 Cl2 N4 O3 Zn2' _chemical_formula_weight 654.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 17.3944(17) _cell_length_b 14.6134(14) _cell_length_c 11.9982(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3049.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2998 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 24.97 _exptl_crystal_description Needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 1.780 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.715 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS 2.03 (Sheldrick, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 15361 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 25.05 _reflns_number_total 5355 _reflns_number_gt 4507 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SHELXS-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0872P)^2^] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.165(17) _refine_ls_number_reflns 5355 _refine_ls_number_parameters 326 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1269 _refine_ls_wR_factor_gt 0.1212 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 Zn1 Zn 0.90086(4) 0.17832(4) 0.32113(7) 0.03094(18) Uani 1 1 d . . . Zn2 Zn 0.87040(3) 0.38856(4) 0.37156(6) 0.02938(17) Uani 1 1 d . . . Cl1 Cl 0.92555(8) 0.10346(9) 0.48781(10) 0.0284(3) Uani 1 1 d . . . Cl2 Cl 0.87356(7) 0.51418(8) 0.25076(11) 0.0229(3) Uani 1 1 d . . . O1 O 0.81250(19) 0.2707(2) 0.3650(4) 0.0342(9) Uani 1 1 d . . . O2 O 0.9491(2) 0.2997(3) 0.3027(4) 0.0378(10) Uani 1 1 d . . . O3 O 0.7743(5) -0.1663(5) 0.6605(8) 0.094(2) Uani 1 1 d . . . N1 N 0.8068(3) 0.0985(3) 0.2460(4) 0.0341(12) Uani 1 1 d . . . N2 N 0.9727(3) 0.0855(3) 0.2122(5) 0.0394(13) Uani 1 1 d . . . N3 N 0.7720(3) 0.4473(3) 0.4750(4) 0.0324(11) Uani 1 1 d . . . N4 N 0.9342(3) 0.4197(3) 0.5204(4) 0.0330(11) Uani 1 1 d . . . C1 C 0.5743(3) 0.2514(4) 0.3529(6) 0.0356(15) Uani 1 1 d . . . C2 C 0.6101(3) 0.3037(4) 0.4337(6) 0.0346(14) Uani 1 1 d . . . H2A H 0.5793 0.3353 0.4866 0.041 Uiso 1 1 calc R . . C3 C 0.6900(3) 0.3115(4) 0.4401(5) 0.0306(13) Uani 1 1 d . . . C4 C 0.7356(3) 0.2643(4) 0.3609(5) 0.0316(13) Uani 1 1 d . . . C5 C 0.7001(3) 0.2101(4) 0.2810(5) 0.0305(13) Uani 1 1 d . . . C6 C 0.6211(3) 0.2044(4) 0.2776(5) 0.0344(14) Uani 1 1 d . . . H6A H 0.5976 0.1672 0.2223 0.041 Uiso 1 1 calc R . . C7 C 0.4876(3) 0.2443(5) 0.3464(6) 0.0470(19) Uani 1 1 d . . . H7A H 0.4645 0.2816 0.4054 0.070 Uiso 1 1 calc R . . H7B H 0.4721 0.1803 0.3559 0.070 Uiso 1 1 calc R . . H7C H 0.4701 0.2664 0.2736 0.070 Uiso 1 1 calc R . . C8 C 0.7470(4) 0.1596(4) 0.1964(5) 0.0368(14) Uani 1 1 d . . . H8A H 0.7121 0.1221 0.1497 0.044 Uiso 1 1 calc R . . H8B H 0.7725 0.2046 0.1470 0.044 Uiso 1 1 calc R . . C9 C 0.7706(4) 0.0377(4) 0.3259(7) 0.0481(17) Uani 1 1 d . . . H9A H 0.7292 0.0036 0.2891 0.072 Uiso 1 1 calc R . . H9B H 0.7491 0.0737 0.3874 0.072 Uiso 1 1 calc R . . H9C H 0.8088 -0.0053 0.3551 0.072 Uiso 1 1 calc R . . C10 C 0.8427(4) 0.0432(5) 0.1535(6) 0.0487(17) Uani 1 1 d . . . H10A H 0.8088 -0.0091 0.1349 0.058 Uiso 1 1 calc R . . H10B H 0.8479 0.0818 0.0861 0.058 Uiso 1 1 calc R . . C11 C 0.9203(4) 0.0081(5) 0.1876(6) 0.0473(17) Uani 1 1 d . . . H11A H 0.9150 -0.0310 0.2545 0.057 Uiso 1 1 calc R . . H11B H 0.9421 -0.0296 0.1268 0.057 Uiso 1 1 calc R . . C12 C 0.9954(5) 0.1260(5) 0.1054(6) 0.0506(18) Uani 1 1 d . . . H12A H 1.0262 0.0818 0.0632 0.076 Uiso 1 1 calc R . . H12B H 1.0258 0.1813 0.1190 0.076 Uiso 1 1 calc R . . H12C H 0.9493 0.1419 0.0627 0.076 Uiso 1 1 calc R . . C13 C 1.0423(4) 0.0479(5) 0.2675(6) 0.0493(17) Uani 1 1 d . . . H13A H 1.0702 0.0087 0.2150 0.074 Uiso 1 1 calc R . . H13B H 1.0270 0.0119 0.3327 0.074 Uiso 1 1 calc R . . H13C H 1.0756 0.0984 0.2912 0.074 Uiso 1 1 calc R . . C14 C 0.7292(4) 0.3687(4) 0.5260(5) 0.0349(14) Uani 1 1 d . . . H14A H 0.7657 0.3301 0.5684 0.042 Uiso 1 1 calc R . . H14B H 0.6905 0.3926 0.5789 0.042 Uiso 1 1 calc R . . C15 C 0.7168(4) 0.5097(5) 0.4193(6) 0.0434(16) Uani 1 1 d . . . H15A H 0.6778 0.5295 0.4731 0.065 Uiso 1 1 calc R . . H15B H 0.6918 0.4775 0.3574 0.065 Uiso 1 1 calc R . . H15C H 0.7443 0.5633 0.3906 0.065 Uiso 1 1 calc R . . C16 C 0.8128(4) 0.5003(4) 0.5629(5) 0.0395(15) Uani 1 1 d . . . H16A H 0.7765 0.5143 0.6241 0.047 Uiso 1 1 calc R . . H16B H 0.8308 0.5590 0.5311 0.047 Uiso 1 1 calc R . . C17 C 0.8812(4) 0.4486(5) 0.6098(6) 0.0413(16) Uani 1 1 d . . . H17A H 0.9090 0.4883 0.6632 0.050 Uiso 1 1 calc R . . H17B H 0.8628 0.3941 0.6508 0.050 Uiso 1 1 calc R . . C18 C 0.9879(4) 0.4946(5) 0.4909(6) 0.0431(15) Uani 1 1 d . . . H18A H 1.0185 0.5112 0.5565 0.065 Uiso 1 1 calc R . . H18B H 0.9586 0.5479 0.4656 0.065 Uiso 1 1 calc R . . H18C H 1.0223 0.4741 0.4311 0.065 Uiso 1 1 calc R . . C19 C 0.9803(4) 0.3426(5) 0.5594(6) 0.0495(18) Uani 1 1 d . . . H19A H 1.0081 0.3603 0.6271 0.074 Uiso 1 1 calc R . . H19B H 1.0173 0.3252 0.5014 0.074 Uiso 1 1 calc R . . H19C H 0.9466 0.2906 0.5758 0.074 Uiso 1 1 calc R . . C20 C 1.0074(4) 0.3354(5) 0.2354(7) 0.0491(18) Uani 1 1 d . . . H20A H 1.0011 0.4025 0.2301 0.059 Uiso 1 1 calc R . . H20B H 1.0024 0.3097 0.1594 0.059 Uiso 1 1 calc R . . C21 C 1.0867(4) 0.3141(5) 0.2797(8) 0.058(2) Uani 1 1 d . . . H21A H 1.1255 0.3402 0.2296 0.087 Uiso 1 1 calc R . . H21B H 1.0936 0.2477 0.2840 0.087 Uiso 1 1 calc R . . H21C H 1.0926 0.3408 0.3542 0.087 Uiso 1 1 calc R . . C22 C 0.7912(6) -0.1750(9) 0.5469(11) 0.100(4) Uani 1 1 d . . . H22A H 0.8264 -0.2272 0.5341 0.120 Uiso 1 1 calc R . . H22B H 0.8158 -0.1186 0.5185 0.120 Uiso 1 1 calc R . . C23 C 0.7162(8) -0.1908(13) 0.4902(11) 0.148(7) Uani 1 1 d . . . H23A H 0.6935 -0.1324 0.4645 0.178 Uiso 1 1 calc R . . H23B H 0.7224 -0.2321 0.4254 0.178 Uiso 1 1 calc R . . C24 C 0.6687(7) -0.2327(8) 0.5749(11) 0.100(4) Uani 1 1 d . . . H24A H 0.6577 -0.2972 0.5554 0.120 Uiso 1 1 calc R . . H24B H 0.6194 -0.1995 0.5820 0.120 Uiso 1 1 calc R . . C25 C 0.7118(6) -0.2279(8) 0.6785(12) 0.096(4) Uani 1 1 d . . . H25A H 0.6785 -0.2052 0.7395 0.115 Uiso 1 1 calc R . . H25B H 0.7313 -0.2892 0.6992 0.115 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 Zn1 0.0329(3) 0.0292(3) 0.0307(3) 0.0006(3) 0.0014(3) 0.0033(3) Zn2 0.0322(3) 0.0281(3) 0.0278(3) 0.0004(3) -0.0017(3) -0.0039(3) Cl1 0.0434(8) 0.0277(7) 0.0142(6) 0.0059(5) -0.0014(6) 0.0112(6) Cl2 0.0258(6) 0.0250(6) 0.0180(6) 0.0082(5) -0.0003(5) -0.0048(5) O1 0.0223(19) 0.0258(19) 0.054(3) -0.006(2) -0.0004(19) -0.0027(15) O2 0.034(2) 0.037(2) 0.042(3) 0.000(2) 0.009(2) -0.0067(17) O3 0.086(5) 0.094(5) 0.103(6) -0.003(4) -0.017(4) -0.016(4) N1 0.040(3) 0.029(3) 0.033(3) 0.001(2) 0.003(2) 0.001(2) N2 0.045(3) 0.031(3) 0.043(3) -0.006(2) 0.008(2) 0.007(2) N3 0.035(3) 0.033(3) 0.029(3) -0.005(2) 0.004(2) 0.001(2) N4 0.035(3) 0.033(3) 0.031(3) -0.001(2) -0.010(2) -0.001(2) C1 0.029(3) 0.031(3) 0.048(4) 0.010(3) -0.004(3) -0.003(2) C2 0.033(3) 0.028(3) 0.043(4) -0.002(3) 0.008(3) 0.002(2) C3 0.034(3) 0.024(3) 0.033(3) 0.002(2) 0.003(3) 0.000(2) C4 0.030(3) 0.027(3) 0.037(3) 0.006(3) 0.003(3) -0.001(2) C5 0.036(3) 0.028(3) 0.028(3) 0.005(2) 0.002(2) -0.005(2) C6 0.038(3) 0.027(3) 0.038(4) 0.000(3) -0.005(3) -0.002(3) C7 0.026(3) 0.055(4) 0.061(6) 0.009(3) -0.003(3) -0.003(3) C8 0.040(3) 0.035(3) 0.036(4) -0.002(3) -0.003(3) 0.010(3) C9 0.049(4) 0.034(3) 0.062(5) 0.010(3) 0.014(4) 0.001(3) C10 0.053(4) 0.038(4) 0.055(5) -0.026(3) 0.000(3) -0.001(3) C11 0.052(4) 0.033(4) 0.057(5) -0.009(3) 0.003(3) 0.012(3) C12 0.069(5) 0.046(4) 0.037(4) 0.005(3) 0.007(4) 0.010(4) C13 0.050(4) 0.046(4) 0.052(4) -0.004(3) -0.001(3) 0.010(3) C14 0.036(3) 0.037(3) 0.032(3) 0.000(3) 0.004(3) -0.004(3) C15 0.043(4) 0.041(4) 0.046(4) 0.002(3) 0.003(3) 0.000(3) C16 0.040(4) 0.041(4) 0.038(4) -0.008(3) 0.004(3) -0.009(3) C17 0.048(4) 0.041(4) 0.035(4) -0.004(3) 0.005(3) -0.015(3) C18 0.046(4) 0.044(4) 0.039(4) 0.002(3) -0.009(3) -0.015(3) C19 0.057(4) 0.054(4) 0.038(4) 0.003(3) -0.017(3) 0.003(3) C20 0.050(4) 0.043(4) 0.055(5) 0.001(3) 0.013(3) 0.001(3) C21 0.050(4) 0.050(4) 0.073(6) -0.003(4) -0.003(4) 0.009(3) C22 0.075(7) 0.138(11) 0.087(9) 0.006(8) 0.007(6) -0.015(7) C23 0.099(9) 0.28(2) 0.066(8) 0.000(10) -0.012(7) -0.063(11) C24 0.087(8) 0.094(8) 0.121(10) -0.030(7) 0.004(8) -0.033(6) C25 0.070(6) 0.081(7) 0.137(11) -0.015(7) -0.007(7) -0.021(6) _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 Zn1 O2 1.975(4) . ? Zn1 O1 2.112(4) . ? Zn1 N1 2.202(5) . ? Zn1 N2 2.261(5) . ? Zn1 Cl1 2.3197(15) . ? Zn2 O1 1.997(3) . ? Zn2 O2 2.060(4) . ? Zn2 N4 2.151(5) . ? Zn2 N3 2.282(5) . ? Zn2 Cl2 2.3396(13) . ? O1 C4 1.342(6) . ? O2 C20 1.396(8) . ? O3 C22 1.399(15) . ? O3 C25 1.428(13) . ? N1 C9 1.452(8) . ? N1 C8 1.494(8) . ? N1 C10 1.508(8) . ? N2 C12 1.465(9) . ? N2 C11 1.482(9) . ? N2 C13 1.486(9) . ? N3 C15 1.482(8) . ? N3 C16 1.489(8) . ? N3 C14 1.499(8) . ? N4 C19 1.460(8) . ? N4 C17 1.477(8) . ? N4 C18 1.483(8) . ? C1 C2 1.382(9) . ? C1 C6 1.397(9) . ? C1 C7 1.513(8) . ? C2 C3 1.398(8) . ? C3 C4 1.415(9) . ? C3 C14 1.492(9) . ? C4 C5 1.389(8) . ? C5 C6 1.378(8) . ? C5 C8 1.497(9) . ? C10 C11 1.501(10) . ? C16 C17 1.516(9) . ? C20 C21 1.511(10) . ? C22 C23 1.489(16) . ? C23 C24 1.444(18) . ? C24 C25 1.453(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 O1 76.31(15) . . ? O2 Zn1 N1 138.22(18) . . ? O1 Zn1 N1 84.27(16) . . ? O2 Zn1 N2 103.84(18) . . ? O1 Zn1 N2 158.42(19) . . ? N1 Zn1 N2 81.72(19) . . ? O2 Zn1 Cl1 116.19(14) . . ? O1 Zn1 Cl1 102.77(14) . . ? N1 Zn1 Cl1 103.93(14) . . ? N2 Zn1 Cl1 96.50(15) . . ? O1 Zn2 O2 77.06(15) . . ? O1 Zn2 N4 118.36(19) . . ? O2 Zn2 N4 97.06(18) . . ? O1 Zn2 N3 88.13(17) . . ? O2 Zn2 N3 162.55(17) . . ? N4 Zn2 N3 81.75(18) . . ? O1 Zn2 Cl2 131.64(14) . . ? O2 Zn2 Cl2 103.32(13) . . ? N4 Zn2 Cl2 109.66(14) . . ? N3 Zn2 Cl2 93.39(13) . . ? C4 O1 Zn2 124.3(3) . . ? C4 O1 Zn1 132.2(3) . . ? Zn2 O1 Zn1 101.19(15) . . ? C20 O2 Zn1 135.1(4) . . ? C20 O2 Zn2 118.6(4) . . ? Zn1 O2 Zn2 103.79(17) . . ? C22 O3 C25 104.5(9) . . ? C9 N1 C8 109.0(5) . . ? C9 N1 C10 109.7(5) . . ? C8 N1 C10 108.4(5) . . ? C9 N1 Zn1 112.1(4) . . ? C8 N1 Zn1 111.4(4) . . ? C10 N1 Zn1 106.2(4) . . ? C12 N2 C11 107.4(5) . . ? C12 N2 C13 108.7(6) . . ? C11 N2 C13 108.0(5) . . ? C12 N2 Zn1 114.3(4) . . ? C11 N2 Zn1 103.5(4) . . ? C13 N2 Zn1 114.5(4) . . ? C15 N3 C16 108.0(5) . . ? C15 N3 C14 109.5(5) . . ? C16 N3 C14 110.2(5) . . ? C15 N3 Zn2 118.2(4) . . ? C16 N3 Zn2 102.8(4) . . ? C14 N3 Zn2 107.8(4) . . ? C19 N4 C17 109.4(5) . . ? C19 N4 C18 107.4(5) . . ? C17 N4 C18 110.8(5) . . ? C19 N4 Zn2 112.7(4) . . ? C17 N4 Zn2 110.0(4) . . ? C18 N4 Zn2 106.4(4) . . ? C2 C1 C6 117.6(5) . . ? C2 C1 C7 121.5(6) . . ? C6 C1 C7 120.9(6) . . ? C1 C2 C3 122.1(6) . . ? C2 C3 C4 118.7(5) . . ? C2 C3 C14 122.6(5) . . ? C4 C3 C14 118.7(5) . . ? O1 C4 C5 120.5(5) . . ? O1 C4 C3 120.0(5) . . ? C5 C4 C3 119.5(5) . . ? C6 C5 C4 119.9(6) . . ? C6 C5 C8 119.6(5) . . ? C4 C5 C8 120.5(5) . . ? C5 C6 C1 122.2(6) . . ? N1 C8 C5 113.8(5) . . ? C11 C10 N1 110.8(6) . . ? N2 C11 C10 110.3(5) . . ? C3 C14 N3 111.9(5) . . ? N3 C16 C17 112.3(5) . . ? N4 C17 C16 111.2(5) . . ? O2 C20 C21 112.5(6) . . ? O3 C22 C23 106.0(10) . . ? C24 C23 C22 104.2(11) . . ? C23 C24 C25 106.7(10) . . ? O3 C25 C24 107.1(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.986 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.099 data_II _database_code_depnum_ccdc_archive 'CCDC 272408' _audit_creation_method SHELXL-97 _chemical_name_systematic ; LCo2Cl3OEt ; _chemical_name_common CMC077A _chemical_compound_source 'Laurie E. Breyfogle' _chemical_melting_point ? _chemical_formula_moiety 'C21 H40 Cl2 Co2 N4 O2' _chemical_formula_sum 'C21 H40 Cl2 Co2 N4 O2' _chemical_formula_weight 569.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.0998 0.0984 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3050 0.6296 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.0961(15) _cell_length_b 11.4544(14) _cell_length_c 16.2755(15) _cell_angle_alpha 90.00 _cell_angle_beta 106.145(5) _cell_angle_gamma 90.00 _cell_volume 2524.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3631 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 21.257 _exptl_crystal_description needle _exptl_crystal_colour pink _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 0.806 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9762 _exptl_absorpt_correction_T_max 0.9856 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_special_details 'L. Breyfogel / Prof. W. Tolman' _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.5500 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator 'diamond [111]' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27494 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 20.31 _reflns_number_total 4932 _reflns_number_gt 4549 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+2.4803P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4932 _refine_ls_number_parameters 288 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0668 _refine_ls_wR_factor_gt 0.0654 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 Co1 Co 0.561500(16) 0.63286(2) 0.304047(14) 0.00895(7) Uani 1 1 d . . . Co2 Co 0.414351(16) 0.53794(2) 0.141251(14) 0.00966(7) Uani 1 1 d . . . Cl1 Cl 0.46631(3) 0.72376(4) 0.37932(3) 0.01947(11) Uani 1 1 d . . . Cl2 Cl 0.35099(3) 0.61355(4) 0.00259(3) 0.01843(11) Uani 1 1 d . . . O1 O 0.51741(9) 0.47439(10) 0.24948(8) 0.0110(2) Uani 1 1 d . . . O2 O 0.48407(9) 0.68448(11) 0.18792(8) 0.0131(3) Uani 1 1 d . . . N1 N 0.64694(11) 0.54299(13) 0.42000(9) 0.0110(3) Uani 1 1 d . . . N2 N 0.70745(11) 0.65753(13) 0.29168(9) 0.0117(3) Uani 1 1 d . . . N3 N 0.38535(11) 0.35395(13) 0.09873(9) 0.0126(3) Uani 1 1 d . . . N4 N 0.28120(11) 0.51550(14) 0.17821(10) 0.0157(3) Uani 1 1 d . . . C1 C 0.55395(12) 0.13562(15) 0.35136(11) 0.0124(3) Uani 1 1 d . . . C2 C 0.51878(12) 0.15561(15) 0.26370(11) 0.0117(3) Uani 1 1 d . . . H2A H 0.5018 0.0906 0.2263 0.014 Uiso 1 1 calc R . . C3 C 0.50758(12) 0.26780(15) 0.22894(11) 0.0102(3) Uani 1 1 d . . . C4 C 0.52942(12) 0.36621(14) 0.28276(11) 0.0093(3) Uani 1 1 d . . . C5 C 0.56462(12) 0.34742(15) 0.37184(11) 0.0104(3) Uani 1 1 d . . . C6 C 0.57610(12) 0.23359(16) 0.40363(11) 0.0123(3) Uani 1 1 d . . . H6A H 0.6001 0.2225 0.4637 0.015 Uiso 1 1 calc R . . C7 C 0.56692(15) 0.01403(16) 0.38764(13) 0.0188(4) Uani 1 1 d . . . H7A H 0.5311 -0.0413 0.3441 0.028 Uiso 1 1 calc R . . H7B H 0.5408 0.0102 0.4374 0.028 Uiso 1 1 calc R . . H7C H 0.6373 -0.0060 0.4050 0.028 Uiso 1 1 calc R . . C8 C 0.58445(13) 0.44582(15) 0.43578(11) 0.0126(3) Uani 1 1 d . . . H8A H 0.5202 0.4788 0.4377 0.015 Uiso 1 1 calc R . . H8B H 0.6165 0.4128 0.4930 0.015 Uiso 1 1 calc R . . C9 C 0.67296(14) 0.61730(16) 0.49734(12) 0.0172(4) Uani 1 1 d . . . H9A H 0.7140 0.5726 0.5456 0.026 Uiso 1 1 calc R . . H9B H 0.6125 0.6426 0.5106 0.026 Uiso 1 1 calc R . . H9C H 0.7097 0.6858 0.4870 0.026 Uiso 1 1 calc R . . C10 C 0.73732(13) 0.50288(16) 0.40038(11) 0.0135(3) Uani 1 1 d . . . H10A H 0.7213 0.4389 0.3579 0.016 Uiso 1 1 calc R . . H10B H 0.7849 0.4728 0.4529 0.016 Uiso 1 1 calc R . . C11 C 0.78268(13) 0.60466(16) 0.36481(11) 0.0134(3) Uani 1 1 d . . . H11A H 0.8069 0.6640 0.4100 0.016 Uiso 1 1 calc R . . H11B H 0.8395 0.5770 0.3456 0.016 Uiso 1 1 calc R . . C12 C 0.70696(14) 0.59737(19) 0.21116(12) 0.0204(4) Uani 1 1 d . . . H12A H 0.7705 0.6096 0.1990 0.031 Uiso 1 1 calc R . . H12B H 0.6537 0.6290 0.1642 0.031 Uiso 1 1 calc R . . H12C H 0.6963 0.5136 0.2170 0.031 Uiso 1 1 calc R . . C13 C 0.72926(14) 0.78264(17) 0.28453(13) 0.0189(4) Uani 1 1 d . . . H13A H 0.7941 0.7910 0.2740 0.028 Uiso 1 1 calc R . . H13B H 0.7296 0.8226 0.3378 0.028 Uiso 1 1 calc R . . H13C H 0.6785 0.8173 0.2369 0.028 Uiso 1 1 calc R . . C14 C 0.47545(13) 0.28121(16) 0.13353(11) 0.0130(3) Uani 1 1 d . . . H14A H 0.5305 0.3162 0.1153 0.016 Uiso 1 1 calc R . . H14B H 0.4631 0.2026 0.1075 0.016 Uiso 1 1 calc R . . C15 C 0.35847(15) 0.33974(18) 0.00489(12) 0.0197(4) Uani 1 1 d . . . H15A H 0.3471 0.2569 -0.0096 0.030 Uiso 1 1 calc R . . H15B H 0.4123 0.3688 -0.0168 0.030 Uiso 1 1 calc R . . H15C H 0.2982 0.3841 -0.0212 0.030 Uiso 1 1 calc R . . C16 C 0.30147(13) 0.31521(17) 0.13051(12) 0.0167(4) Uani 1 1 d . . . H16A H 0.3264 0.2879 0.1904 0.020 Uiso 1 1 calc R . . H16B H 0.2668 0.2494 0.0953 0.020 Uiso 1 1 calc R . . C17 C 0.23048(13) 0.41595(17) 0.12585(12) 0.0175(4) Uani 1 1 d . . . H17A H 0.2038 0.4411 0.0656 0.021 Uiso 1 1 calc R . . H17B H 0.1744 0.3901 0.1469 0.021 Uiso 1 1 calc R . . C18 C 0.29769(15) 0.4900(2) 0.27008(13) 0.0229(4) Uani 1 1 d . . . H18A H 0.2341 0.4760 0.2817 0.034 Uiso 1 1 calc R . . H18B H 0.3306 0.5566 0.3040 0.034 Uiso 1 1 calc R . . H18C H 0.3394 0.4205 0.2854 0.034 Uiso 1 1 calc R . . C19 C 0.21754(15) 0.62075(18) 0.15702(15) 0.0244(4) Uani 1 1 d . . . H19A H 0.1550 0.6062 0.1705 0.037 Uiso 1 1 calc R . . H19B H 0.2044 0.6382 0.0959 0.037 Uiso 1 1 calc R . . H19C H 0.2512 0.6872 0.1906 0.037 Uiso 1 1 calc R . . C20 C 0.44378(15) 0.79795(16) 0.16635(13) 0.0192(4) Uani 1 1 d . . . H20A H 0.4567 0.8457 0.2190 0.023 Uiso 1 1 calc R . . H20B H 0.3713 0.7914 0.1423 0.023 Uiso 1 1 calc R . . C21 C 0.48646(16) 0.85961(18) 0.10218(14) 0.0252(5) Uani 1 1 d . . . H21A H 0.4556 0.9365 0.0889 0.038 Uiso 1 1 calc R . . H21B H 0.4735 0.8131 0.0497 0.038 Uiso 1 1 calc R . . H21C H 0.5579 0.8690 0.1265 0.038 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 Co1 0.00853(12) 0.00885(12) 0.00916(12) -0.00021(8) 0.00192(9) -0.00023(8) Co2 0.00853(12) 0.01096(13) 0.00840(12) 0.00151(8) 0.00056(9) -0.00128(8) Cl1 0.0245(2) 0.0158(2) 0.0220(2) 0.00087(17) 0.01282(19) 0.00623(18) Cl2 0.0223(2) 0.0180(2) 0.0119(2) 0.00438(16) -0.00027(18) -0.00147(18) O1 0.0126(6) 0.0093(6) 0.0094(6) 0.0010(4) 0.0003(5) -0.0019(5) O2 0.0140(6) 0.0101(6) 0.0129(6) 0.0019(5) 0.0001(5) -0.0007(5) N1 0.0132(7) 0.0108(7) 0.0087(7) -0.0017(5) 0.0024(6) -0.0025(6) N2 0.0114(7) 0.0146(7) 0.0082(7) -0.0003(6) 0.0012(6) -0.0018(6) N3 0.0133(7) 0.0139(7) 0.0085(7) 0.0006(6) -0.0003(6) -0.0017(6) N4 0.0127(7) 0.0187(8) 0.0163(8) -0.0011(6) 0.0052(6) -0.0034(6) C1 0.0094(8) 0.0119(8) 0.0154(9) 0.0019(7) 0.0029(7) -0.0002(6) C2 0.0097(8) 0.0114(8) 0.0137(8) -0.0024(7) 0.0027(7) -0.0016(6) C3 0.0081(7) 0.0124(8) 0.0097(8) 0.0000(6) 0.0020(6) -0.0010(6) C4 0.0061(7) 0.0100(8) 0.0119(8) 0.0005(6) 0.0025(6) -0.0007(6) C5 0.0085(7) 0.0119(8) 0.0110(8) 0.0000(6) 0.0029(6) -0.0011(6) C6 0.0098(8) 0.0154(9) 0.0110(8) 0.0022(7) 0.0015(6) -0.0017(7) C7 0.0225(10) 0.0123(9) 0.0186(9) 0.0033(7) 0.0011(8) -0.0015(7) C8 0.0168(8) 0.0119(8) 0.0101(8) 0.0003(7) 0.0054(7) -0.0023(7) C9 0.0220(9) 0.0166(9) 0.0112(8) -0.0055(7) 0.0016(7) -0.0052(7) C10 0.0113(8) 0.0132(8) 0.0136(8) 0.0004(7) -0.0003(7) 0.0006(7) C11 0.0098(8) 0.0167(9) 0.0120(8) 0.0009(7) 0.0003(7) -0.0006(7) C12 0.0162(9) 0.0355(11) 0.0115(9) -0.0064(8) 0.0069(7) 0.0007(8) C13 0.0151(9) 0.0168(9) 0.0227(10) 0.0062(7) 0.0017(8) -0.0039(7) C14 0.0147(8) 0.0141(8) 0.0097(8) -0.0023(7) 0.0024(7) -0.0010(7) C15 0.0265(10) 0.0204(10) 0.0087(8) -0.0024(7) -0.0011(8) -0.0012(8) C16 0.0125(8) 0.0180(9) 0.0180(9) 0.0003(7) 0.0014(7) -0.0062(7) C17 0.0117(8) 0.0201(9) 0.0182(9) 0.0008(7) -0.0001(7) -0.0050(7) C18 0.0196(10) 0.0361(12) 0.0159(9) -0.0018(8) 0.0096(8) -0.0079(9) C19 0.0177(9) 0.0223(10) 0.0371(12) 0.0007(9) 0.0138(9) 0.0035(8) C20 0.0236(10) 0.0118(9) 0.0186(9) 0.0025(7) -0.0002(8) 0.0030(7) C21 0.0245(10) 0.0182(10) 0.0278(11) 0.0084(8) -0.0012(9) -0.0036(8) _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 Co1 O2 1.9915(12) . ? Co1 O1 2.0403(12) . ? Co1 N2 2.1409(15) . ? Co1 N1 2.1926(15) . ? Co1 Cl1 2.3021(5) . ? Co2 O2 1.9862(13) . ? Co2 O1 2.0784(12) . ? Co2 N4 2.1398(15) . ? Co2 N3 2.2203(15) . ? Co2 Cl2 2.3495(5) . ? O1 C4 1.344(2) . ? O2 C20 1.423(2) . ? N1 C10 1.470(2) . ? N1 C9 1.479(2) . ? N1 C8 1.486(2) . ? N2 C13 1.477(2) . ? N2 C12 1.479(2) . ? N2 C11 1.485(2) . ? N3 C15 1.477(2) . ? N3 C16 1.484(2) . ? N3 C14 1.493(2) . ? N4 C18 1.477(2) . ? N4 C17 1.483(2) . ? N4 C19 1.485(3) . ? C1 C6 1.390(3) . ? C1 C2 1.393(2) . ? C1 C7 1.504(2) . ? C2 C3 1.395(2) . ? C2 H2A 0.9500 . ? C3 C4 1.408(2) . ? C3 C14 1.500(2) . ? C4 C5 1.412(2) . ? C5 C6 1.395(2) . ? C5 C8 1.506(2) . ? C6 H6A 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.520(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.515(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.517(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 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 O2 Co1 O1 80.26(5) . . ? O2 Co1 N2 99.15(5) . . ? O1 Co1 N2 105.12(5) . . ? O2 Co1 N1 168.86(5) . . ? O1 Co1 N1 89.14(5) . . ? N2 Co1 N1 80.25(6) . . ? O2 Co1 Cl1 97.13(4) . . ? O1 Co1 Cl1 118.81(4) . . ? N2 Co1 Cl1 135.07(4) . . ? N1 Co1 Cl1 90.93(4) . . ? O2 Co2 O1 79.45(5) . . ? O2 Co2 N4 111.93(6) . . ? O1 Co2 N4 100.41(6) . . ? O2 Co2 N3 161.79(5) . . ? O1 Co2 N3 87.51(5) . . ? N4 Co2 N3 82.75(6) . . ? O2 Co2 Cl2 94.09(4) . . ? O1 Co2 Cl2 158.84(4) . . ? N4 Co2 Cl2 100.69(5) . . ? N3 Co2 Cl2 93.59(4) . . ? C4 O1 Co1 130.98(11) . . ? C4 O1 Co2 130.12(10) . . ? Co1 O1 Co2 96.54(5) . . ? C20 O2 Co2 123.82(11) . . ? C20 O2 Co1 125.53(11) . . ? Co2 O2 Co1 101.21(5) . . ? C10 N1 C9 109.87(14) . . ? C10 N1 C8 113.24(14) . . ? C9 N1 C8 107.62(13) . . ? C10 N1 Co1 105.16(10) . . ? C9 N1 Co1 114.16(11) . . ? C8 N1 Co1 106.88(10) . . ? C13 N2 C12 109.39(15) . . ? C13 N2 C11 109.93(14) . . ? C12 N2 C11 110.27(14) . . ? C13 N2 Co1 111.22(11) . . ? C12 N2 Co1 104.71(11) . . ? C11 N2 Co1 111.19(11) . . ? C15 N3 C16 109.10(14) . . ? C15 N3 C14 106.11(14) . . ? C16 N3 C14 112.16(14) . . ? C15 N3 Co2 113.52(11) . . ? C16 N3 Co2 105.70(11) . . ? C14 N3 Co2 110.37(10) . . ? C18 N4 C17 110.16(15) . . ? C18 N4 C19 108.09(16) . . ? C17 N4 C19 109.09(15) . . ? C18 N4 Co2 113.88(12) . . ? C17 N4 Co2 104.55(11) . . ? C19 N4 Co2 110.97(12) . . ? C6 C1 C2 116.71(16) . . ? C6 C1 C7 121.68(16) . . ? C2 C1 C7 121.61(16) . . ? C1 C2 C3 122.32(16) . . ? C1 C2 H2A 118.8 . . ? C3 C2 H2A 118.8 . . ? C2 C3 C4 120.30(15) . . ? C2 C3 C14 118.80(15) . . ? C4 C3 C14 120.86(15) . . ? O1 C4 C3 120.41(15) . . ? O1 C4 C5 121.54(15) . . ? C3 C4 C5 118.06(15) . . ? C6 C5 C4 119.63(16) . . ? C6 C5 C8 117.57(15) . . ? C4 C5 C8 122.68(15) . . ? C1 C6 C5 122.97(16) . . ? C1 C6 H6A 118.5 . . ? C5 C6 H6A 118.5 . . ? C1 C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C5 116.50(14) . . ? N1 C8 H8A 108.2 . . ? C5 C8 H8A 108.2 . . ? N1 C8 H8B 108.2 . . ? C5 C8 H8B 108.2 . . ? H8A C8 H8B 107.3 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 C11 108.95(14) . . ? N1 C10 H10A 109.9 . . ? C11 C10 H10A 109.9 . . ? N1 C10 H10B 109.9 . . ? C11 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? N2 C11 C10 109.62(14) . . ? N2 C11 H11A 109.7 . . ? C10 C11 H11A 109.7 . . ? N2 C11 H11B 109.7 . . ? C10 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? N2 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 H13A 109.5 . . ? N2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C14 C3 115.48(14) . . ? N3 C14 H14A 108.4 . . ? C3 C14 H14A 108.4 . . ? N3 C14 H14B 108.4 . . ? C3 C14 H14B 108.4 . . ? H14A C14 H14B 107.5 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 C17 109.51(15) . . ? N3 C16 H16A 109.8 . . ? C17 C16 H16A 109.8 . . ? N3 C16 H16B 109.8 . . ? C17 C16 H16B 109.8 . . ? H16A C16 H16B 108.2 . . ? N4 C17 C16 110.53(15) . . ? N4 C17 H17A 109.5 . . ? C16 C17 H17A 109.5 . . ? N4 C17 H17B 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? N4 C18 H18A 109.5 . . ? N4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N4 C19 H19A 109.5 . . ? N4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O2 C20 C21 112.81(16) . . ? O2 C20 H20A 109.0 . . ? C21 C20 H20A 109.0 . . ? O2 C20 H20B 109.0 . . ? C21 C20 H20B 109.0 . . ? H20A C20 H20B 107.8 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? 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 O2 Co1 O1 C4 -175.28(14) . . . . ? N2 Co1 O1 C4 87.79(14) . . . . ? N1 Co1 O1 C4 8.13(14) . . . . ? Cl1 Co1 O1 C4 -82.46(14) . . . . ? O2 Co1 O1 Co2 -11.79(5) . . . . ? N2 Co1 O1 Co2 -108.73(6) . . . . ? N1 Co1 O1 Co2 171.62(5) . . . . ? Cl1 Co1 O1 Co2 81.03(5) . . . . ? O2 Co2 O1 C4 175.56(14) . . . . ? N4 Co2 O1 C4 64.95(14) . . . . ? N3 Co2 O1 C4 -17.21(14) . . . . ? Cl2 Co2 O1 C4 -110.72(14) . . . . ? O2 Co2 O1 Co1 11.86(5) . . . . ? N4 Co2 O1 Co1 -98.75(6) . . . . ? N3 Co2 O1 Co1 179.09(6) . . . . ? Cl2 Co2 O1 Co1 85.58(11) . . . . ? O1 Co2 O2 C20 -160.07(14) . . . . ? N4 Co2 O2 C20 -63.00(14) . . . . ? N3 Co2 O2 C20 154.97(17) . . . . ? Cl2 Co2 O2 C20 40.25(13) . . . . ? O1 Co2 O2 Co1 -12.31(5) . . . . ? N4 Co2 O2 Co1 84.77(7) . . . . ? N3 Co2 O2 Co1 -57.26(19) . . . . ? Cl2 Co2 O2 Co1 -171.98(4) . . . . ? O1 Co1 O2 C20 159.52(14) . . . . ? N2 Co1 O2 C20 -96.57(14) . . . . ? N1 Co1 O2 C20 177.5(2) . . . . ? Cl1 Co1 O2 C20 41.39(14) . . . . ? O1 Co1 O2 Co2 12.51(5) . . . . ? N2 Co1 O2 Co2 116.42(6) . . . . ? N1 Co1 O2 Co2 30.4(3) . . . . ? Cl1 Co1 O2 Co2 -105.61(5) . . . . ? O2 Co1 N1 C10 60.9(3) . . . . ? O1 Co1 N1 C10 78.58(11) . . . . ? N2 Co1 N1 C10 -26.93(10) . . . . ? Cl1 Co1 N1 C10 -162.62(10) . . . . ? O2 Co1 N1 C9 -178.6(2) . . . . ? O1 Co1 N1 C9 -160.92(12) . . . . ? N2 Co1 N1 C9 93.57(12) . . . . ? Cl1 Co1 N1 C9 -42.12(12) . . . . ? O2 Co1 N1 C8 -59.7(3) . . . . ? O1 Co1 N1 C8 -42.05(11) . . . . ? N2 Co1 N1 C8 -147.56(11) . . . . ? Cl1 Co1 N1 C8 76.75(10) . . . . ? O2 Co1 N2 C13 67.70(12) . . . . ? O1 Co1 N2 C13 149.99(11) . . . . ? N1 Co1 N2 C13 -123.58(12) . . . . ? Cl1 Co1 N2 C13 -42.14(14) . . . . ? O2 Co1 N2 C12 -50.35(12) . . . . ? O1 Co1 N2 C12 31.95(12) . . . . ? N1 Co1 N2 C12 118.38(12) . . . . ? Cl1 Co1 N2 C12 -160.18(10) . . . . ? O2 Co1 N2 C11 -169.43(11) . . . . ? O1 Co1 N2 C11 -87.13(11) . . . . ? N1 Co1 N2 C11 -0.70(11) . . . . ? Cl1 Co1 N2 C11 80.74(12) . . . . ? O2 Co2 N3 C15 -103.51(19) . . . . ? O1 Co2 N3 C15 -147.56(12) . . . . ? N4 Co2 N3 C15 111.61(13) . . . . ? Cl2 Co2 N3 C15 11.28(12) . . . . ? O2 Co2 N3 C16 136.94(16) . . . . ? O1 Co2 N3 C16 92.90(11) . . . . ? N4 Co2 N3 C16 -7.93(11) . . . . ? Cl2 Co2 N3 C16 -108.26(10) . . . . ? O2 Co2 N3 C14 15.5(2) . . . . ? O1 Co2 N3 C14 -28.59(11) . . . . ? N4 Co2 N3 C14 -129.42(12) . . . . ? Cl2 Co2 N3 C14 130.25(10) . . . . ? O2 Co2 N4 C18 -69.79(14) . . . . ? O1 Co2 N4 C18 12.93(14) . . . . ? N3 Co2 N4 C18 99.04(14) . . . . ? Cl2 Co2 N4 C18 -168.66(13) . . . . ? O2 Co2 N4 C17 169.92(10) . . . . ? O1 Co2 N4 C17 -107.36(11) . . . . ? N3 Co2 N4 C17 -21.26(11) . . . . ? Cl2 Co2 N4 C17 71.05(11) . . . . ? O2 Co2 N4 C19 52.44(14) . . . . ? O1 Co2 N4 C19 135.16(13) . . . . ? N3 Co2 N4 C19 -138.74(13) . . . . ? Cl2 Co2 N4 C19 -46.43(13) . . . . ? C6 C1 C2 C3 1.1(2) . . . . ? C7 C1 C2 C3 -179.12(17) . . . . ? C1 C2 C3 C4 -1.8(3) . . . . ? C1 C2 C3 C14 176.10(15) . . . . ? Co1 O1 C4 C3 -168.72(11) . . . . ? Co2 O1 C4 C3 33.0(2) . . . . ? Co1 O1 C4 C5 10.8(2) . . . . ? Co2 O1 C4 C5 -147.48(13) . . . . ? C2 C3 C4 O1 -179.10(15) . . . . ? C14 C3 C4 O1 3.1(2) . . . . ? C2 C3 C4 C5 1.3(2) . . . . ? C14 C3 C4 C5 -176.50(15) . . . . ? O1 C4 C5 C6 -179.91(15) . . . . ? C3 C4 C5 C6 -0.3(2) . . . . ? O1 C4 C5 C8 4.3(2) . . . . ? C3 C4 C5 C8 -176.18(15) . . . . ? C2 C1 C6 C5 -0.1(3) . . . . ? C7 C1 C6 C5 -179.85(17) . . . . ? C4 C5 C6 C1 -0.3(3) . . . . ? C8 C5 C6 C1 175.76(16) . . . . ? C10 N1 C8 C5 -47.6(2) . . . . ? C9 N1 C8 C5 -169.26(15) . . . . ? Co1 N1 C8 C5 67.71(16) . . . . ? C6 C5 C8 N1 133.34(17) . . . . ? C4 C5 C8 N1 -50.7(2) . . . . ? C9 N1 C10 C11 -73.09(17) . . . . ? C8 N1 C10 C11 166.54(14) . . . . ? Co1 N1 C10 C11 50.20(15) . . . . ? C13 N2 C11 C10 151.58(15) . . . . ? C12 N2 C11 C10 -87.73(18) . . . . ? Co1 N2 C11 C10 27.96(17) . . . . ? N1 C10 C11 N2 -53.40(18) . . . . ? C15 N3 C14 C3 -171.17(15) . . . . ? C16 N3 C14 C3 -52.1(2) . . . . ? Co2 N3 C14 C3 65.45(16) . . . . ? C2 C3 C14 N3 124.59(17) . . . . ? C4 C3 C14 N3 -57.6(2) . . . . ? C15 N3 C16 C17 -86.59(18) . . . . ? C14 N3 C16 C17 156.15(15) . . . . ? Co2 N3 C16 C17 35.83(16) . . . . ? C18 N4 C17 C16 -74.30(19) . . . . ? C19 N4 C17 C16 167.20(16) . . . . ? Co2 N4 C17 C16 48.45(16) . . . . ? N3 C16 C17 N4 -59.33(19) . . . . ? Co2 O2 C20 C21 -102.31(17) . . . . ? Co1 O2 C20 C21 117.71(15) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 20.31 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.418 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.063 data_III _database_code_depnum_ccdc_archive 'CCDC 272409' _audit_creation_method SHELXL-97 _chemical_name_systematic ; LMg2Cl2OEt ; _chemical_name_common 03196 _chemical_compound_source 'Laurie E. Breyfogle' _chemical_melting_point ? _chemical_formula_moiety 'C23 H46 Cl2 Mg2 N4 O3, C1 CH2 Cl2' _chemical_formula_sum 'C24 H48 Cl4 Mg2 N4 O3' _chemical_formula_weight 631.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.544(2) _cell_length_b 10.6347(14) _cell_length_c 15.894(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.778(2) _cell_angle_gamma 90.00 _cell_volume 3267.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5795 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description square _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.283 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 0.431 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.902360 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25064 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.06 _reflns_number_total 5795 _reflns_number_gt 4191 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL, Bruker' _computing_publication_material 'Bruker, SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+3.9053P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5795 _refine_ls_number_parameters 345 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0744 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1397 _refine_ls_wR_factor_gt 0.1229 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.90700(5) 0.17563(8) 0.26146(5) 0.0381(2) Uani 1 1 d . . . Cl3 Cl 0.53225(6) 0.74788(10) -0.19526(8) 0.0615(3) Uani 1 1 d . . . Cl4 Cl 0.58674(9) 0.50554(16) -0.21850(13) 0.1169(7) Uani 1 1 d . . . Cl2 Cl 0.74096(4) -0.17852(7) -0.01122(6) 0.0381(2) Uani 1 1 d . . . Mg1 Mg 0.86613(5) 0.23196(9) 0.10848(6) 0.0219(2) Uani 1 1 d . . . Mg2 Mg 0.74935(5) 0.04511(9) 0.02546(7) 0.0258(2) Uani 1 1 d . . . N1 N 0.85918(12) 0.4424(2) 0.11624(17) 0.0263(6) Uani 1 1 d . . . N2 N 0.96487(13) 0.2889(2) 0.08758(17) 0.0273(6) Uani 1 1 d . . . N3 N 0.63694(13) 0.0651(2) 0.01603(18) 0.0307(6) Uani 1 1 d . . . N4 N 0.70143(13) 0.1000(2) -0.12042(17) 0.0307(6) Uani 1 1 d . . . O1 O 0.76188(10) 0.22849(18) 0.07183(13) 0.0236(4) Uani 1 1 d . . . O2 O 0.84797(10) 0.07778(18) 0.03608(13) 0.0252(5) Uani 1 1 d . . . O3 O 0.77575(13) -0.0019(2) 0.16859(16) 0.0415(6) Uani 1 1 d D . . H3B H 0.8081(14) 0.046(3) 0.202(2) 0.050 Uiso 1 1 d D . . C1 C 0.71587(15) 0.3158(3) 0.07528(19) 0.0234(6) Uani 1 1 d . . . C2 C 0.65212(15) 0.2825(3) 0.08403(19) 0.0247(6) Uani 1 1 d . . . C3 C 0.60617(15) 0.3764(3) 0.0893(2) 0.0289(7) Uani 1 1 d . . . H3A H 0.5633 0.3522 0.0949 0.035 Uiso 1 1 calc R . . C4 C 0.62063(16) 0.5035(3) 0.0867(2) 0.0304(7) Uani 1 1 d . . . C5 C 0.68273(16) 0.5355(3) 0.0756(2) 0.0289(7) Uani 1 1 d . . . H5A H 0.6937 0.6218 0.0727 0.035 Uiso 1 1 calc R . . C6 C 0.72937(15) 0.4445(3) 0.06845(19) 0.0249(6) Uani 1 1 d . . . C7 C 0.57168(18) 0.6037(3) 0.0983(3) 0.0432(9) Uani 1 1 d . . . H7A H 0.5269 0.5653 0.0921 0.065 Uiso 1 1 calc R . . H7B H 0.5653 0.6688 0.0526 0.065 Uiso 1 1 calc R . . H7C H 0.5913 0.6416 0.1578 0.065 Uiso 1 1 calc R . . C8 C 0.79318(15) 0.4860(3) 0.0491(2) 0.0280(7) Uani 1 1 d . . . H8A H 0.7904 0.4537 -0.0105 0.034 Uiso 1 1 calc R . . H8B H 0.7937 0.5789 0.0464 0.034 Uiso 1 1 calc R . . C9 C 0.86247(17) 0.4831(3) 0.2065(2) 0.0352(8) Uani 1 1 d . . . H9A H 0.8536 0.5736 0.2061 0.053 Uiso 1 1 calc R . . H9B H 0.9085 0.4648 0.2494 0.053 Uiso 1 1 calc R . . H9C H 0.8275 0.4377 0.2239 0.053 Uiso 1 1 calc R . . C10 C 0.91786(16) 0.5002(3) 0.0950(2) 0.0344(8) Uani 1 1 d . . . H10A H 0.9290 0.5833 0.1244 0.041 Uiso 1 1 calc R . . H10B H 0.9045 0.5130 0.0296 0.041 Uiso 1 1 calc R . . C11 C 0.98052(16) 0.4164(3) 0.1267(2) 0.0335(8) Uani 1 1 d . . . H11A H 1.0184 0.4539 0.1096 0.040 Uiso 1 1 calc R . . H11B H 0.9964 0.4103 0.1927 0.040 Uiso 1 1 calc R . . C12 C 1.02431(17) 0.2066(3) 0.1322(3) 0.0414(9) Uani 1 1 d . . . H12A H 1.0661 0.2414 0.1245 0.062 Uiso 1 1 calc R . . H12B H 1.0155 0.1224 0.1057 0.062 Uiso 1 1 calc R . . H12C H 1.0308 0.2012 0.1961 0.062 Uiso 1 1 calc R . . C13 C 0.95380(19) 0.2927(3) -0.0096(2) 0.0399(8) Uani 1 1 d . . . H13A H 0.9947 0.3285 -0.0191 0.060 Uiso 1 1 calc R . . H13B H 0.9133 0.3449 -0.0400 0.060 Uiso 1 1 calc R . . H13C H 0.9460 0.2072 -0.0340 0.060 Uiso 1 1 calc R . . C14 C 0.63206(16) 0.1474(3) 0.0893(2) 0.0314(7) Uani 1 1 d . . . H14A H 0.6621 0.1122 0.1470 0.038 Uiso 1 1 calc R . . H14B H 0.5839 0.1451 0.0892 0.038 Uiso 1 1 calc R . . C15 C 0.60717(18) -0.0579(3) 0.0277(3) 0.0428(9) Uani 1 1 d . . . H15A H 0.5588 -0.0466 0.0231 0.064 Uiso 1 1 calc R . . H15B H 0.6334 -0.0924 0.0866 0.064 Uiso 1 1 calc R . . H15C H 0.6097 -0.1161 -0.0189 0.064 Uiso 1 1 calc R . . C16 C 0.59883(17) 0.1176(3) -0.0733(2) 0.0370(8) Uani 1 1 d . . . H16A H 0.6024 0.2104 -0.0710 0.044 Uiso 1 1 calc R . . H16B H 0.5493 0.0949 -0.0904 0.044 Uiso 1 1 calc R . . C17 C 0.62763(17) 0.0678(3) -0.1433(2) 0.0367(8) Uani 1 1 d . . . H17A H 0.6221 -0.0247 -0.1477 0.044 Uiso 1 1 calc R . . H17B H 0.6012 0.1042 -0.2023 0.044 Uiso 1 1 calc R . . C18 C 0.73193(19) 0.0268(4) -0.1768(2) 0.0437(9) Uani 1 1 d . . . H18A H 0.7096 0.0506 -0.2396 0.065 Uiso 1 1 calc R . . H18B H 0.7249 -0.0631 -0.1697 0.065 Uiso 1 1 calc R . . H18C H 0.7816 0.0445 -0.1586 0.065 Uiso 1 1 calc R . . C19 C 0.7100(2) 0.2347(3) -0.1373(2) 0.0456(9) Uani 1 1 d . . . H19A H 0.6873 0.2528 -0.2010 0.068 Uiso 1 1 calc R . . H19B H 0.7594 0.2545 -0.1200 0.068 Uiso 1 1 calc R . . H19C H 0.6891 0.2860 -0.1021 0.068 Uiso 1 1 calc R . . C20 C 0.89150(16) -0.0178(3) 0.0235(2) 0.0338(8) Uani 1 1 d . . . H20A H 0.9284 0.0211 0.0052 0.041 Uiso 1 1 calc R . . H20B H 0.8642 -0.0737 -0.0255 0.041 Uiso 1 1 calc R . . C21 C 0.92427(19) -0.0952(3) 0.1064(3) 0.0465(9) Uani 1 1 d . . . H21A H 0.9595 -0.1505 0.0974 0.070 Uiso 1 1 calc R . . H21B H 0.8887 -0.1463 0.1186 0.070 Uiso 1 1 calc R . . H21C H 0.9459 -0.0394 0.1573 0.070 Uiso 1 1 calc R . . C22 C 0.5928(2) 0.6304(4) -0.1463(3) 0.0680(13) Uani 1 1 d . . . H22A H 0.6399 0.6664 -0.1286 0.082 Uiso 1 1 calc R . . H22B H 0.5852 0.5994 -0.0916 0.082 Uiso 1 1 calc R . . C23 C 0.7859(2) -0.1163(4) 0.2169(3) 0.0546(10) Uani 1 1 d . . . H23A H 0.8309 -0.1532 0.2199 0.066 Uiso 1 1 calc R . . H23B H 0.7491 -0.1765 0.1849 0.066 Uiso 1 1 calc R . . C24 C 0.7849(3) -0.0973(5) 0.3112(3) 0.0823(16) Uani 1 1 d . . . H24A H 0.7954 -0.1770 0.3439 0.124 Uiso 1 1 calc R . . H24B H 0.7389 -0.0682 0.3085 0.124 Uiso 1 1 calc R . . H24C H 0.8196 -0.0343 0.3420 0.124 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 Cl1 0.0480(5) 0.0398(5) 0.0218(4) 0.0042(3) 0.0056(4) -0.0010(4) Cl3 0.0537(6) 0.0537(6) 0.0713(7) -0.0064(5) 0.0136(5) -0.0119(5) Cl4 0.0938(11) 0.0895(11) 0.1436(15) -0.0577(11) 0.0090(10) 0.0170(9) Cl2 0.0409(5) 0.0236(4) 0.0479(5) -0.0026(4) 0.0126(4) -0.0023(3) Mg1 0.0217(5) 0.0223(5) 0.0208(5) -0.0009(4) 0.0059(4) -0.0014(4) Mg2 0.0245(5) 0.0224(5) 0.0286(6) -0.0023(4) 0.0066(4) -0.0016(4) N1 0.0236(13) 0.0268(13) 0.0288(14) -0.0011(11) 0.0091(11) -0.0026(11) N2 0.0241(13) 0.0308(14) 0.0270(14) 0.0000(11) 0.0087(11) -0.0010(11) N3 0.0266(14) 0.0282(14) 0.0355(16) -0.0022(12) 0.0081(12) -0.0038(11) N4 0.0311(14) 0.0328(15) 0.0248(14) -0.0014(11) 0.0049(12) -0.0017(12) O1 0.0242(10) 0.0212(10) 0.0248(11) 0.0002(8) 0.0075(9) 0.0002(8) O2 0.0250(11) 0.0237(11) 0.0265(11) -0.0036(9) 0.0080(9) 0.0018(8) O3 0.0464(15) 0.0385(14) 0.0353(14) 0.0054(11) 0.0083(12) -0.0033(11) C1 0.0235(15) 0.0266(16) 0.0180(15) -0.0005(12) 0.0044(12) 0.0024(12) C2 0.0260(16) 0.0273(15) 0.0194(15) -0.0001(12) 0.0057(12) -0.0008(13) C3 0.0221(15) 0.0367(18) 0.0279(17) 0.0002(14) 0.0086(13) 0.0014(13) C4 0.0306(17) 0.0337(17) 0.0252(17) 0.0007(14) 0.0070(14) 0.0059(14) C5 0.0309(17) 0.0240(16) 0.0280(17) 0.0014(13) 0.0050(14) 0.0020(13) C6 0.0255(15) 0.0252(15) 0.0227(16) 0.0010(12) 0.0067(13) -0.0001(12) C7 0.037(2) 0.039(2) 0.056(2) -0.0035(17) 0.0185(18) 0.0096(16) C8 0.0292(17) 0.0214(15) 0.0340(18) 0.0036(13) 0.0115(14) 0.0002(13) C9 0.0336(18) 0.0366(18) 0.0334(19) -0.0104(15) 0.0086(15) -0.0035(15) C10 0.0317(18) 0.0291(17) 0.046(2) -0.0020(15) 0.0173(16) -0.0099(14) C11 0.0274(17) 0.0334(18) 0.040(2) -0.0041(15) 0.0111(15) -0.0090(14) C12 0.0254(17) 0.043(2) 0.052(2) 0.0003(17) 0.0080(16) 0.0031(15) C13 0.048(2) 0.043(2) 0.035(2) -0.0006(16) 0.0227(17) -0.0050(17) C14 0.0295(17) 0.0310(17) 0.0369(19) -0.0015(14) 0.0156(15) -0.0030(13) C15 0.0343(19) 0.0340(19) 0.064(3) -0.0114(17) 0.0212(18) -0.0123(15) C16 0.0273(17) 0.042(2) 0.0353(19) -0.0052(16) 0.0029(15) 0.0032(15) C17 0.0294(17) 0.042(2) 0.0313(18) -0.0062(15) 0.0007(14) -0.0013(15) C18 0.044(2) 0.060(2) 0.0264(19) -0.0011(17) 0.0105(16) 0.0054(18) C19 0.058(2) 0.045(2) 0.0276(19) 0.0037(16) 0.0073(17) -0.0063(18) C20 0.0285(17) 0.0342(18) 0.039(2) -0.0085(15) 0.0125(15) 0.0020(14) C21 0.044(2) 0.038(2) 0.056(2) 0.0030(18) 0.0162(19) 0.0161(17) C22 0.063(3) 0.069(3) 0.056(3) -0.008(2) -0.001(2) -0.002(2) C23 0.069(3) 0.038(2) 0.060(3) 0.0099(19) 0.027(2) -0.001(2) C24 0.097(4) 0.094(4) 0.062(3) 0.017(3) 0.036(3) 0.022(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 Mg1 2.3652(13) . ? Cl3 C22 1.749(5) . ? Cl4 C22 1.731(5) . ? Cl2 Mg2 2.4408(13) . ? Mg1 O2 1.965(2) . ? Mg1 O1 2.021(2) . ? Mg1 N2 2.247(3) . ? Mg1 N1 2.249(3) . ? Mg1 Mg2 3.0502(14) . ? Mg2 O2 2.006(2) . ? Mg2 O1 2.070(2) . ? Mg2 O3 2.210(3) . ? Mg2 N4 2.267(3) . ? Mg2 N3 2.273(3) . ? N1 C9 1.478(4) . ? N1 C8 1.488(4) . ? N1 C10 1.490(4) . ? N2 C12 1.475(4) . ? N2 C11 1.481(4) . ? N2 C13 1.484(4) . ? N3 C16 1.479(4) . ? N3 C15 1.482(4) . ? N3 C14 1.487(4) . ? N4 C17 1.475(4) . ? N4 C18 1.477(4) . ? N4 C19 1.479(4) . ? O1 C1 1.339(3) . ? O2 C20 1.412(4) . ? O3 C23 1.416(4) . ? O3 H3B 0.863(5) . ? C1 C2 1.408(4) . ? C1 C6 1.409(4) . ? C2 C3 1.395(4) . ? C2 C14 1.505(4) . ? C3 C4 1.388(5) . ? C3 H3A 0.9500 . ? C4 C5 1.388(4) . ? C4 C7 1.519(4) . ? C5 C6 1.393(4) . ? C5 H5A 0.9500 . ? C6 C8 1.510(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.505(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.522(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.506(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.520(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 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 O2 Mg1 O1 80.98(8) . . ? O2 Mg1 N2 98.08(9) . . ? O1 Mg1 N2 152.15(10) . . ? O2 Mg1 N1 149.27(10) . . ? O1 Mg1 N1 87.32(9) . . ? N2 Mg1 N1 79.45(9) . . ? O2 Mg1 Cl1 108.77(8) . . ? O1 Mg1 Cl1 105.35(7) . . ? N2 Mg1 Cl1 101.31(8) . . ? N1 Mg1 Cl1 101.70(8) . . ? O2 Mg1 Mg2 40.30(6) . . ? O1 Mg1 Mg2 42.40(6) . . ? N2 Mg1 Mg2 136.81(8) . . ? N1 Mg1 Mg2 128.09(7) . . ? Cl1 Mg1 Mg2 103.50(4) . . ? O2 Mg2 O1 78.84(8) . . ? O2 Mg2 O3 93.64(9) . . ? O1 Mg2 O3 83.62(9) . . ? O2 Mg2 N4 96.78(10) . . ? O1 Mg2 N4 94.61(9) . . ? O3 Mg2 N4 168.89(11) . . ? O2 Mg2 N3 164.62(10) . . ? O1 Mg2 N3 86.36(9) . . ? O3 Mg2 N3 88.80(10) . . ? N4 Mg2 N3 80.13(10) . . ? O2 Mg2 Cl2 100.17(7) . . ? O1 Mg2 Cl2 173.36(8) . . ? O3 Mg2 Cl2 89.91(8) . . ? N4 Mg2 Cl2 92.02(8) . . ? N3 Mg2 Cl2 95.01(8) . . ? O2 Mg2 Mg1 39.32(6) . . ? O1 Mg2 Mg1 41.17(6) . . ? O3 Mg2 Mg1 79.57(7) . . ? N4 Mg2 Mg1 106.29(8) . . ? N3 Mg2 Mg1 126.90(8) . . ? Cl2 Mg2 Mg1 136.03(5) . . ? C9 N1 C8 109.7(2) . . ? C9 N1 C10 109.0(2) . . ? C8 N1 C10 108.7(2) . . ? C9 N1 Mg1 111.18(19) . . ? C8 N1 Mg1 109.25(17) . . ? C10 N1 Mg1 109.05(18) . . ? C12 N2 C11 108.4(2) . . ? C12 N2 C13 109.1(3) . . ? C11 N2 C13 110.3(3) . . ? C12 N2 Mg1 114.2(2) . . ? C11 N2 Mg1 105.28(18) . . ? C13 N2 Mg1 109.46(19) . . ? C16 N3 C15 110.3(3) . . ? C16 N3 C14 112.0(3) . . ? C15 N3 C14 106.4(2) . . ? C16 N3 Mg2 107.14(19) . . ? C15 N3 Mg2 111.2(2) . . ? C14 N3 Mg2 109.85(18) . . ? C17 N4 C18 109.9(3) . . ? C17 N4 C19 110.8(3) . . ? C18 N4 C19 107.4(3) . . ? C17 N4 Mg2 104.31(19) . . ? C18 N4 Mg2 111.0(2) . . ? C19 N4 Mg2 113.4(2) . . ? C1 O1 Mg1 132.03(18) . . ? C1 O1 Mg2 131.55(18) . . ? Mg1 O1 Mg2 96.42(9) . . ? C20 O2 Mg1 132.80(19) . . ? C20 O2 Mg2 122.25(18) . . ? Mg1 O2 Mg2 100.37(9) . . ? C23 O3 Mg2 133.8(2) . . ? C23 O3 H3B 103(3) . . ? Mg2 O3 H3B 112(3) . . ? O1 C1 C2 121.5(3) . . ? O1 C1 C6 120.7(3) . . ? C2 C1 C6 117.7(3) . . ? C3 C2 C1 119.8(3) . . ? C3 C2 C14 118.4(3) . . ? C1 C2 C14 121.8(3) . . ? C4 C3 C2 122.6(3) . . ? C4 C3 H3A 118.7 . . ? C2 C3 H3A 118.7 . . ? C3 C4 C5 117.2(3) . . ? C3 C4 C7 121.5(3) . . ? C5 C4 C7 121.2(3) . . ? C4 C5 C6 121.8(3) . . ? C4 C5 H5A 119.1 . . ? C6 C5 H5A 119.1 . . ? C5 C6 C1 120.7(3) . . ? C5 C6 C8 118.8(3) . . ? C1 C6 C8 120.4(3) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C6 114.0(2) . . ? N1 C8 H8A 108.8 . . ? C6 C8 H8A 108.8 . . ? N1 C8 H8B 108.8 . . ? C6 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 C11 110.3(3) . . ? N1 C10 H10A 109.6 . . ? C11 C10 H10A 109.6 . . ? N1 C10 H10B 109.6 . . ? C11 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? N2 C11 C10 111.2(3) . . ? N2 C11 H11A 109.4 . . ? C10 C11 H11A 109.4 . . ? N2 C11 H11B 109.4 . . ? C10 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? N2 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 H13A 109.5 . . ? N2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C14 C2 115.3(3) . . ? N3 C14 H14A 108.5 . . ? C2 C14 H14A 108.5 . . ? N3 C14 H14B 108.5 . . ? C2 C14 H14B 108.5 . . ? H14A C14 H14B 107.5 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 C17 111.1(3) . . ? N3 C16 H16A 109.4 . . ? C17 C16 H16A 109.4 . . ? N3 C16 H16B 109.4 . . ? C17 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? N4 C17 C16 111.1(3) . . ? N4 C17 H17A 109.4 . . ? C16 C17 H17A 109.4 . . ? N4 C17 H17B 109.4 . . ? C16 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? N4 C18 H18A 109.5 . . ? N4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N4 C19 H19A 109.5 . . ? N4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O2 C20 C21 112.8(3) . . ? O2 C20 H20A 109.0 . . ? C21 C20 H20A 109.0 . . ? O2 C20 H20B 109.0 . . ? C21 C20 H20B 109.0 . . ? H20A C20 H20B 107.8 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Cl4 C22 Cl3 111.9(2) . . ? Cl4 C22 H22A 109.2 . . ? Cl3 C22 H22A 109.2 . . ? Cl4 C22 H22B 109.2 . . ? Cl3 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? O3 C23 C24 111.8(4) . . ? O3 C23 H23A 109.3 . . ? C24 C23 H23A 109.3 . . ? O3 C23 H23B 109.3 . . ? C24 C23 H23B 109.3 . . ? H23A C23 H23B 107.9 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 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 O1 Mg1 Mg2 O2 158.70(13) . . . . ? N2 Mg1 Mg2 O2 20.18(14) . . . . ? N1 Mg1 Mg2 O2 139.85(14) . . . . ? Cl1 Mg1 Mg2 O2 -103.21(10) . . . . ? O2 Mg1 Mg2 O1 -158.70(13) . . . . ? N2 Mg1 Mg2 O1 -138.52(14) . . . . ? N1 Mg1 Mg2 O1 -18.84(12) . . . . ? Cl1 Mg1 Mg2 O1 98.09(9) . . . . ? O2 Mg1 Mg2 O3 109.07(12) . . . . ? O1 Mg1 Mg2 O3 -92.24(11) . . . . ? N2 Mg1 Mg2 O3 129.24(13) . . . . ? N1 Mg1 Mg2 O3 -111.08(12) . . . . ? Cl1 Mg1 Mg2 O3 5.86(8) . . . . ? O2 Mg1 Mg2 N4 -80.64(12) . . . . ? O1 Mg1 Mg2 N4 78.06(11) . . . . ? N2 Mg1 Mg2 N4 -60.47(14) . . . . ? N1 Mg1 Mg2 N4 59.21(12) . . . . ? Cl1 Mg1 Mg2 N4 176.15(8) . . . . ? O2 Mg1 Mg2 N3 -170.42(14) . . . . ? O1 Mg1 Mg2 N3 -11.72(12) . . . . ? N2 Mg1 Mg2 N3 -150.25(14) . . . . ? N1 Mg1 Mg2 N3 -30.57(14) . . . . ? Cl1 Mg1 Mg2 N3 86.37(10) . . . . ? O2 Mg1 Mg2 Cl2 30.21(11) . . . . ? O1 Mg1 Mg2 Cl2 -171.09(11) . . . . ? N2 Mg1 Mg2 Cl2 50.39(14) . . . . ? N1 Mg1 Mg2 Cl2 170.06(10) . . . . ? Cl1 Mg1 Mg2 Cl2 -73.00(8) . . . . ? O2 Mg1 N1 C9 157.2(2) . . . . ? O1 Mg1 N1 C9 89.86(19) . . . . ? N2 Mg1 N1 C9 -114.8(2) . . . . ? Cl1 Mg1 N1 C9 -15.3(2) . . . . ? Mg2 Mg1 N1 C9 102.46(19) . . . . ? O2 Mg1 N1 C8 36.0(3) . . . . ? O1 Mg1 N1 C8 -31.34(19) . . . . ? N2 Mg1 N1 C8 124.03(19) . . . . ? Cl1 Mg1 N1 C8 -136.46(17) . . . . ? Mg2 Mg1 N1 C8 -18.7(2) . . . . ? O2 Mg1 N1 C10 -82.7(3) . . . . ? O1 Mg1 N1 C10 -150.0(2) . . . . ? N2 Mg1 N1 C10 5.4(2) . . . . ? Cl1 Mg1 N1 C10 104.9(2) . . . . ? Mg2 Mg1 N1 C10 -137.37(18) . . . . ? O2 Mg1 N2 C12 -70.0(2) . . . . ? O1 Mg1 N2 C12 -155.9(2) . . . . ? N1 Mg1 N2 C12 141.1(2) . . . . ? Cl1 Mg1 N2 C12 41.1(2) . . . . ? Mg2 Mg1 N2 C12 -83.0(2) . . . . ? O2 Mg1 N2 C11 171.28(19) . . . . ? O1 Mg1 N2 C11 85.3(3) . . . . ? N1 Mg1 N2 C11 22.33(19) . . . . ? Cl1 Mg1 N2 C11 -77.63(19) . . . . ? Mg2 Mg1 N2 C11 158.26(16) . . . . ? O2 Mg1 N2 C13 52.7(2) . . . . ? O1 Mg1 N2 C13 -33.3(3) . . . . ? N1 Mg1 N2 C13 -96.3(2) . . . . ? Cl1 Mg1 N2 C13 163.78(19) . . . . ? Mg2 Mg1 N2 C13 39.7(2) . . . . ? O2 Mg2 N3 C16 72.3(4) . . . . ? O1 Mg2 N3 C16 88.0(2) . . . . ? O3 Mg2 N3 C16 171.7(2) . . . . ? N4 Mg2 N3 C16 -7.3(2) . . . . ? Cl2 Mg2 N3 C16 -98.52(19) . . . . ? Mg1 Mg2 N3 C16 95.7(2) . . . . ? O2 Mg2 N3 C15 -167.1(3) . . . . ? O1 Mg2 N3 C15 -151.4(2) . . . . ? O3 Mg2 N3 C15 -67.7(2) . . . . ? N4 Mg2 N3 C15 113.2(2) . . . . ? Cl2 Mg2 N3 C15 22.1(2) . . . . ? Mg1 Mg2 N3 C15 -143.7(2) . . . . ? O2 Mg2 N3 C14 -49.6(5) . . . . ? O1 Mg2 N3 C14 -33.9(2) . . . . ? O3 Mg2 N3 C14 49.8(2) . . . . ? N4 Mg2 N3 C14 -129.3(2) . . . . ? Cl2 Mg2 N3 C14 139.56(19) . . . . ? Mg1 Mg2 N3 C14 -26.2(2) . . . . ? O2 Mg2 N4 C17 173.86(19) . . . . ? O1 Mg2 N4 C17 -106.85(19) . . . . ? O3 Mg2 N4 C17 -26.5(6) . . . . ? N3 Mg2 N4 C17 -21.37(19) . . . . ? Cl2 Mg2 N4 C17 73.37(19) . . . . ? Mg1 Mg2 N4 C17 -147.11(18) . . . . ? O2 Mg2 N4 C18 55.6(2) . . . . ? O1 Mg2 N4 C18 134.9(2) . . . . ? O3 Mg2 N4 C18 -144.8(5) . . . . ? N3 Mg2 N4 C18 -139.7(2) . . . . ? Cl2 Mg2 N4 C18 -44.9(2) . . . . ? Mg1 Mg2 N4 C18 94.6(2) . . . . ? O2 Mg2 N4 C19 -65.4(2) . . . . ? O1 Mg2 N4 C19 13.9(2) . . . . ? O3 Mg2 N4 C19 94.2(6) . . . . ? N3 Mg2 N4 C19 99.3(2) . . . . ? Cl2 Mg2 N4 C19 -165.9(2) . . . . ? Mg1 Mg2 N4 C19 -26.4(2) . . . . ? O2 Mg1 O1 C1 -165.6(2) . . . . ? N2 Mg1 O1 C1 -75.3(3) . . . . ? N1 Mg1 O1 C1 -14.1(2) . . . . ? Cl1 Mg1 O1 C1 87.3(2) . . . . ? Mg2 Mg1 O1 C1 -179.3(3) . . . . ? O2 Mg1 O1 Mg2 13.76(9) . . . . ? N2 Mg1 O1 Mg2 104.0(2) . . . . ? N1 Mg1 O1 Mg2 165.26(9) . . . . ? Cl1 Mg1 O1 Mg2 -93.35(8) . . . . ? O2 Mg2 O1 C1 165.8(2) . . . . ? O3 Mg2 O1 C1 -99.2(2) . . . . ? N4 Mg2 O1 C1 69.8(2) . . . . ? N3 Mg2 O1 C1 -10.0(2) . . . . ? Cl2 Mg2 O1 C1 -112.2(6) . . . . ? Mg1 Mg2 O1 C1 179.4(3) . . . . ? O2 Mg2 O1 Mg1 -13.57(9) . . . . ? O3 Mg2 O1 Mg1 81.43(10) . . . . ? N4 Mg2 O1 Mg1 -109.59(10) . . . . ? N3 Mg2 O1 Mg1 170.63(10) . . . . ? Cl2 Mg2 O1 Mg1 68.5(7) . . . . ? O1 Mg1 O2 C20 -169.7(3) . . . . ? N2 Mg1 O2 C20 38.4(3) . . . . ? N1 Mg1 O2 C20 121.4(3) . . . . ? Cl1 Mg1 O2 C20 -66.5(3) . . . . ? Mg2 Mg1 O2 C20 -155.3(3) . . . . ? O1 Mg1 O2 Mg2 -14.36(9) . . . . ? N2 Mg1 O2 Mg2 -166.21(10) . . . . ? N1 Mg1 O2 Mg2 -83.3(2) . . . . ? Cl1 Mg1 O2 Mg2 88.88(9) . . . . ? O1 Mg2 O2 C20 172.9(2) . . . . ? O3 Mg2 O2 C20 90.1(2) . . . . ? N4 Mg2 O2 C20 -93.7(2) . . . . ? N3 Mg2 O2 C20 -171.1(4) . . . . ? Cl2 Mg2 O2 C20 -0.4(2) . . . . ? Mg1 Mg2 O2 C20 158.8(3) . . . . ? O1 Mg2 O2 Mg1 14.11(9) . . . . ? O3 Mg2 O2 Mg1 -68.65(10) . . . . ? N4 Mg2 O2 Mg1 107.49(10) . . . . ? N3 Mg2 O2 Mg1 30.1(4) . . . . ? Cl2 Mg2 O2 Mg1 -159.21(7) . . . . ? O2 Mg2 O3 C23 -98.0(3) . . . . ? O1 Mg2 O3 C23 -176.3(3) . . . . ? N4 Mg2 O3 C23 102.3(6) . . . . ? N3 Mg2 O3 C23 97.2(3) . . . . ? Cl2 Mg2 O3 C23 2.2(3) . . . . ? Mg1 Mg2 O3 C23 -134.9(3) . . . . ? Mg1 O1 C1 C2 -151.5(2) . . . . ? Mg2 O1 C1 C2 29.4(4) . . . . ? Mg1 O1 C1 C6 29.7(4) . . . . ? Mg2 O1 C1 C6 -149.4(2) . . . . ? O1 C1 C2 C3 178.6(3) . . . . ? C6 C1 C2 C3 -2.6(4) . . . . ? O1 C1 C2 C14 -0.5(4) . . . . ? C6 C1 C2 C14 178.3(3) . . . . ? C1 C2 C3 C4 -0.3(5) . . . . ? C14 C2 C3 C4 178.8(3) . . . . ? C2 C3 C4 C5 2.0(5) . . . . ? C2 C3 C4 C7 -176.1(3) . . . . ? C3 C4 C5 C6 -0.8(5) . . . . ? C7 C4 C5 C6 177.4(3) . . . . ? C4 C5 C6 C1 -2.1(5) . . . . ? C4 C5 C6 C8 175.1(3) . . . . ? O1 C1 C6 C5 -177.5(3) . . . . ? C2 C1 C6 C5 3.8(4) . . . . ? O1 C1 C6 C8 5.4(4) . . . . ? C2 C1 C6 C8 -173.4(3) . . . . ? C9 N1 C8 C6 -55.1(3) . . . . ? C10 N1 C8 C6 -174.1(3) . . . . ? Mg1 N1 C8 C6 67.0(3) . . . . ? C5 C6 C8 N1 123.9(3) . . . . ? C1 C6 C8 N1 -58.8(4) . . . . ? C9 N1 C10 C11 88.9(3) . . . . ? C8 N1 C10 C11 -151.7(3) . . . . ? Mg1 N1 C10 C11 -32.7(3) . . . . ? C12 N2 C11 C10 -170.9(3) . . . . ? C13 N2 C11 C10 69.8(3) . . . . ? Mg1 N2 C11 C10 -48.3(3) . . . . ? N1 C10 C11 N2 56.4(4) . . . . ? C16 N3 C14 C2 -52.7(3) . . . . ? C15 N3 C14 C2 -173.3(3) . . . . ? Mg2 N3 C14 C2 66.2(3) . . . . ? C3 C2 C14 N3 128.1(3) . . . . ? C1 C2 C14 N3 -52.7(4) . . . . ? C15 N3 C16 C17 -86.0(3) . . . . ? C14 N3 C16 C17 155.7(3) . . . . ? Mg2 N3 C16 C17 35.2(3) . . . . ? C18 N4 C17 C16 167.0(3) . . . . ? C19 N4 C17 C16 -74.5(3) . . . . ? Mg2 N4 C17 C16 47.9(3) . . . . ? N3 C16 C17 N4 -59.2(4) . . . . ? Mg1 O2 C20 C21 67.5(4) . . . . ? Mg2 O2 C20 C21 -83.5(3) . . . . ? Mg2 O3 C23 C24 -165.1(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3B Cl1 0.863(5) 2.373(12) 3.213(3) 165(3) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.919 _refine_diff_density_min -0.477 _refine_diff_density_rms 0.066 data_IV _database_code_depnum_ccdc_archive 'CCDC 272410' _audit_creation_method SHELXL-97 _chemical_name_systematic ; LZn2Cl3 ; _chemical_name_common 02008 _chemical_compound_source 'Charlotte K. Williams' _chemical_melting_point ? _chemical_formula_moiety 'C23 H43 Cl3 N4 O2 Zn2' _chemical_formula_sum 'C23 H43 Cl3 N4 O2 Zn2' _chemical_formula_weight 644.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 17.254(2) _cell_length_b 15.0382(18) _cell_length_c 11.4742(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2977.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3720 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 22.44 _exptl_crystal_description needles _exptl_crystal_colour white _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 1.906 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.805455 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS, R.Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13479 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0699 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.06 _reflns_number_total 4972 _reflns_number_gt 4012 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0531P)^2^+2.3708P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.21(2) _refine_ls_number_reflns 4972 _refine_ls_number_parameters 299 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1150 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.38883(4) 0.11434(4) 0.30134(6) 0.02613(17) Uani 1 1 d . . . Zn2 Zn 0.40510(4) 0.33319(5) 0.25346(7) 0.02807(18) Uani 1 1 d . . . Cl1 Cl 0.37381(10) 0.00588(11) 0.16774(14) 0.0366(4) Uani 1 1 d . . . Cl2 Cl 0.42936(11) 0.38443(12) 0.43485(15) 0.0423(4) Uani 1 1 d . . . Cl3 Cl 0.48812(9) 0.21439(11) 0.19804(17) 0.0393(4) Uani 1 1 d . . . O1 O 0.3310(2) 0.2271(3) 0.2889(4) 0.0285(10) Uani 1 1 d . . . N1 N 0.3097(3) 0.0664(3) 0.4398(5) 0.0285(12) Uani 1 1 d . . . N2 N 0.4749(3) 0.0731(4) 0.4182(5) 0.0302(12) Uani 1 1 d . . . N3 N 0.3050(3) 0.4040(3) 0.1841(5) 0.0319(12) Uani 1 1 d . . . N4 N 0.4698(3) 0.4282(4) 0.1440(4) 0.0322(13) Uani 1 1 d . . . C1 C 0.2530(3) 0.2309(4) 0.2977(6) 0.0253(12) Uani 1 1 d . . . C2 C 0.2146(3) 0.1865(4) 0.3874(6) 0.0253(13) Uani 1 1 d . . . C3 C 0.1349(4) 0.1878(4) 0.3934(6) 0.0302(15) Uani 1 1 d . . . H3A H 0.1097 0.1564 0.4545 0.036 Uiso 1 1 calc R . . C4 C 0.0898(3) 0.2344(4) 0.3116(6) 0.0305(14) Uani 1 1 d . . . C5 C 0.1297(4) 0.2832(4) 0.2280(6) 0.0300(15) Uani 1 1 d . . . H5A H 0.1008 0.3177 0.1739 0.036 Uiso 1 1 calc R . . C6 C 0.2096(3) 0.2836(4) 0.2202(5) 0.0245(14) Uani 1 1 d . . . C8 C 0.2617(4) 0.1432(4) 0.4811(5) 0.0282(15) Uani 1 1 d . . . H8A H 0.2263 0.1222 0.5431 0.034 Uiso 1 1 calc R . . H8B H 0.2965 0.1884 0.5159 0.034 Uiso 1 1 calc R . . C7 C 0.0022(4) 0.2312(5) 0.3158(7) 0.0423(17) Uani 1 1 d . . . H7A H -0.0143 0.1936 0.3810 0.063 Uiso 1 1 calc R . . H7B H -0.0176 0.2065 0.2426 0.063 Uiso 1 1 calc R . . H7C H -0.0181 0.2915 0.3266 0.063 Uiso 1 1 calc R . . C9 C 0.2497(4) 0.3396(4) 0.1310(6) 0.0334(15) Uani 1 1 d . . . H9A H 0.2783 0.3004 0.0766 0.040 Uiso 1 1 calc R . . H9B H 0.2105 0.3726 0.0855 0.040 Uiso 1 1 calc R . . C11 C 0.2585(4) -0.0064(4) 0.3999(6) 0.0375(17) Uani 1 1 d . . . H11A H 0.2246 -0.0249 0.4641 0.056 Uiso 1 1 calc R . . H11B H 0.2901 -0.0570 0.3747 0.056 Uiso 1 1 calc R . . H11C H 0.2267 0.0145 0.3346 0.056 Uiso 1 1 calc R . . C12 C 0.3596(4) 0.0355(5) 0.5362(6) 0.0350(16) Uani 1 1 d . . . H12A H 0.3333 -0.0131 0.5790 0.042 Uiso 1 1 calc R . . H12B H 0.3688 0.0850 0.5915 0.042 Uiso 1 1 calc R . . C13 C 0.4365(4) 0.0024(5) 0.4885(6) 0.0368(16) Uani 1 1 d . . . H13A H 0.4707 -0.0151 0.5539 0.044 Uiso 1 1 calc R . . H13B H 0.4276 -0.0507 0.4392 0.044 Uiso 1 1 calc R . . C14 C 0.5431(4) 0.0326(5) 0.3588(7) 0.0426(18) Uani 1 1 d . . . H14A H 0.5816 0.0149 0.4172 0.064 Uiso 1 1 calc R . . H14B H 0.5662 0.0760 0.3055 0.064 Uiso 1 1 calc R . . H14C H 0.5264 -0.0199 0.3147 0.064 Uiso 1 1 calc R . . C15 C 0.5019(4) 0.1470(5) 0.4933(7) 0.0419(18) Uani 1 1 d . . . H15A H 0.5422 0.1251 0.5464 0.063 Uiso 1 1 calc R . . H15B H 0.4582 0.1701 0.5388 0.063 Uiso 1 1 calc R . . H15C H 0.5232 0.1946 0.4446 0.063 Uiso 1 1 calc R . . C16 C 0.2669(4) 0.4573(4) 0.2748(7) 0.045(2) Uani 1 1 d . . . H16A H 0.2220 0.4880 0.2413 0.067 Uiso 1 1 calc R . . H16B H 0.3036 0.5012 0.3055 0.067 Uiso 1 1 calc R . . H16C H 0.2497 0.4182 0.3381 0.067 Uiso 1 1 calc R . . C17 C 0.3362(4) 0.4622(5) 0.0900(7) 0.046(2) Uani 1 1 d . . . H17A H 0.2993 0.5111 0.0742 0.055 Uiso 1 1 calc R . . H17B H 0.3426 0.4273 0.0176 0.055 Uiso 1 1 calc R . . C18 C 0.4135(4) 0.5005(5) 0.1261(7) 0.0424(18) Uani 1 1 d . . . H18A H 0.4326 0.5414 0.0650 0.051 Uiso 1 1 calc R . . H18B H 0.4074 0.5348 0.1992 0.051 Uiso 1 1 calc R . . C19 C 0.4958(5) 0.3904(5) 0.0313(7) 0.048(2) Uani 1 1 d . . . H19A H 0.5244 0.4357 -0.0125 0.072 Uiso 1 1 calc R . . H19B H 0.4505 0.3713 -0.0138 0.072 Uiso 1 1 calc R . . H19C H 0.5296 0.3392 0.0458 0.072 Uiso 1 1 calc R . . C20 C 0.5389(4) 0.4630(5) 0.2071(7) 0.0468(19) Uani 1 1 d . . . H20A H 0.5668 0.5048 0.1568 0.070 Uiso 1 1 calc R . . H20B H 0.5731 0.4135 0.2278 0.070 Uiso 1 1 calc R . . H20C H 0.5221 0.4937 0.2781 0.070 Uiso 1 1 calc R . . O1S O 0.2760(13) 0.6485(17) -0.103(2) 0.174(7) Uiso 0.561(10) 1 d PD A 1 C2S C 0.3183(16) 0.721(2) -0.013(3) 0.174(11) Uiso 0.561(10) 1 d PD A 1 H2S1 H 0.3735 0.7028 -0.0096 0.209 Uiso 0.561(10) 1 calc PR A 1 H2S2 H 0.3170 0.7786 -0.0537 0.209 Uiso 0.561(10) 1 calc PR A 1 C3S C 0.2972(18) 0.739(3) 0.101(3) 0.188(12) Uiso 0.561(10) 1 d PD A 1 H3S1 H 0.3163 0.7972 0.1284 0.226 Uiso 0.561(10) 1 calc PR A 1 H3S2 H 0.3137 0.6914 0.1560 0.226 Uiso 0.561(10) 1 calc PR A 1 C4S C 0.2071(18) 0.738(2) 0.079(3) 0.184(11) Uiso 0.561(10) 1 d PD A 1 H4S1 H 0.1785 0.7113 0.1448 0.220 Uiso 0.561(10) 1 calc PR A 1 H4S2 H 0.1870 0.7987 0.0637 0.220 Uiso 0.561(10) 1 calc PR A 1 C5S C 0.2036(14) 0.685(2) -0.020(3) 0.156(10) Uiso 0.561(10) 1 d PD A 1 H5S1 H 0.1685 0.7167 -0.0745 0.188 Uiso 0.561(10) 1 calc PR A 1 H5S2 H 0.1753 0.6307 0.0041 0.188 Uiso 0.561(10) 1 calc PR A 1 O6S O 0.2668(18) 0.658(2) -0.053(3) 0.174(7) Uiso 0.439(10) 1 d PD A 2 C7S C 0.3083(19) 0.741(3) -0.129(4) 0.174(11) Uiso 0.439(10) 1 d PD A 2 H7S1 H 0.3042 0.7943 -0.0779 0.209 Uiso 0.439(10) 1 calc PR A 2 H7S2 H 0.3641 0.7263 -0.1319 0.209 Uiso 0.439(10) 1 calc PR A 2 C8S C 0.290(2) 0.772(3) -0.240(3) 0.188(12) Uiso 0.439(10) 1 d PD A 2 H8S1 H 0.3237 0.7445 -0.3002 0.226 Uiso 0.439(10) 1 calc PR A 2 H8S2 H 0.2946 0.8377 -0.2454 0.226 Uiso 0.439(10) 1 calc PR A 2 C9S C 0.204(2) 0.740(3) -0.250(3) 0.184(11) Uiso 0.439(10) 1 d PD A 2 H9S1 H 0.1673 0.7906 -0.2544 0.220 Uiso 0.439(10) 1 calc PR A 2 H9S2 H 0.1960 0.6999 -0.3170 0.220 Uiso 0.439(10) 1 calc PR A 2 C10S C 0.1984(15) 0.695(3) -0.144(3) 0.156(10) Uiso 0.439(10) 1 d PD A 2 H10A H 0.1667 0.6422 -0.1621 0.188 Uiso 0.439(10) 1 calc PR A 2 H10B H 0.1652 0.7339 -0.0954 0.188 Uiso 0.439(10) 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 Zn1 0.0262(3) 0.0292(4) 0.0230(3) 0.0001(3) -0.0007(3) 0.0048(3) Zn2 0.0304(4) 0.0294(4) 0.0244(3) 0.0002(3) -0.0002(3) -0.0062(3) Cl1 0.0411(10) 0.0406(9) 0.0282(8) -0.0110(8) -0.0022(7) 0.0078(7) Cl2 0.0548(11) 0.0464(10) 0.0256(8) -0.0037(8) -0.0016(8) -0.0189(9) Cl3 0.0311(9) 0.0387(9) 0.0481(10) 0.0111(8) 0.0120(8) 0.0042(7) O1 0.018(2) 0.027(2) 0.040(3) 0.0010(19) 0.0025(19) -0.0005(16) N1 0.027(3) 0.028(3) 0.030(3) -0.004(2) 0.003(2) 0.004(2) N2 0.025(3) 0.030(3) 0.035(3) 0.003(3) -0.008(2) 0.001(2) N3 0.031(3) 0.032(3) 0.033(3) -0.002(3) 0.000(2) -0.004(2) N4 0.042(3) 0.029(3) 0.026(3) -0.001(3) 0.004(2) -0.009(3) C1 0.024(3) 0.025(3) 0.027(3) 0.000(3) -0.001(3) 0.001(2) C2 0.026(3) 0.022(3) 0.029(3) -0.005(3) 0.000(3) 0.000(2) C3 0.031(4) 0.028(3) 0.031(4) -0.001(3) 0.006(3) 0.001(3) C4 0.030(3) 0.030(3) 0.032(3) -0.009(3) 0.006(3) -0.001(2) C5 0.031(3) 0.025(3) 0.034(4) -0.007(3) -0.005(3) 0.003(3) C6 0.023(3) 0.025(3) 0.025(3) -0.008(3) -0.001(2) -0.002(2) C8 0.030(4) 0.029(3) 0.026(4) -0.005(3) 0.000(3) 0.006(3) C7 0.033(4) 0.044(4) 0.050(5) -0.001(4) -0.003(3) -0.002(3) C9 0.037(4) 0.029(3) 0.035(4) 0.001(3) -0.005(3) 0.000(3) C11 0.030(4) 0.037(4) 0.045(4) -0.007(3) 0.003(3) 0.001(3) C12 0.035(4) 0.036(4) 0.034(4) 0.008(3) -0.003(3) 0.005(3) C13 0.043(4) 0.034(4) 0.033(4) 0.003(3) -0.001(3) 0.004(3) C14 0.035(4) 0.040(4) 0.052(5) 0.010(4) -0.002(3) 0.013(3) C15 0.044(5) 0.041(4) 0.040(4) -0.003(4) -0.013(3) 0.005(3) C16 0.052(4) 0.037(4) 0.045(5) -0.008(4) 0.004(3) -0.004(3) C17 0.046(5) 0.042(4) 0.051(5) 0.024(4) -0.007(4) 0.000(4) C18 0.040(4) 0.034(4) 0.053(5) 0.012(4) 0.005(3) -0.011(3) C19 0.066(5) 0.035(4) 0.042(4) -0.005(3) 0.015(4) -0.016(4) C20 0.042(4) 0.057(5) 0.042(4) 0.003(4) -0.004(3) -0.022(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.974(4) . ? Zn1 N2 2.094(5) . ? Zn1 N1 2.216(5) . ? Zn1 Cl1 2.2533(17) . ? Zn1 Cl3 2.5698(18) . ? Zn2 O1 2.085(4) . ? Zn2 N3 2.180(5) . ? Zn2 N4 2.206(5) . ? Zn2 Cl2 2.2585(19) . ? Zn2 Cl3 2.3766(18) . ? O1 C1 1.350(6) . ? N1 C12 1.477(8) . ? N1 C11 1.480(8) . ? N1 C8 1.498(8) . ? N2 C15 1.482(9) . ? N2 C14 1.490(9) . ? N2 C13 1.491(8) . ? N3 C16 1.469(9) . ? N3 C9 1.489(8) . ? N3 C17 1.491(9) . ? N4 C18 1.473(9) . ? N4 C19 1.481(9) . ? N4 C20 1.489(8) . ? C1 C2 1.394(9) . ? C1 C6 1.408(8) . ? C2 C3 1.377(8) . ? C2 C8 1.497(9) . ? C3 C4 1.407(10) . ? C4 C5 1.390(9) . ? C4 C7 1.513(8) . ? C5 C6 1.382(9) . ? C6 C9 1.495(9) . ? C12 C13 1.520(10) . ? C17 C18 1.510(10) . ? O1S C5S 1.66(2) . ? O1S C2S 1.67(2) . ? C2S C3S 1.39(3) . ? C3S C4S 1.58(3) . ? C4S C5S 1.39(3) . ? O6S C10S 1.67(3) . ? O6S C7S 1.68(3) . ? C7S C8S 1.39(3) . ? C7S C10S 2.03(4) . ? C8S C9S 1.57(3) . ? C9S C10S 1.39(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 N2 131.3(2) . . ? O1 Zn1 N1 91.11(18) . . ? N2 Zn1 N1 83.2(2) . . ? O1 Zn1 Cl1 120.98(14) . . ? N2 Zn1 Cl1 107.63(16) . . ? N1 Zn1 Cl1 100.47(14) . . ? O1 Zn1 Cl3 78.51(12) . . ? N2 Zn1 Cl3 89.76(15) . . ? N1 Zn1 Cl3 158.76(14) . . ? Cl1 Zn1 Cl3 100.76(7) . . ? O1 Zn2 N3 87.62(17) . . ? O1 Zn2 N4 156.53(19) . . ? N3 Zn2 N4 82.9(2) . . ? O1 Zn2 Cl2 101.24(14) . . ? N3 Zn2 Cl2 108.46(16) . . ? N4 Zn2 Cl2 102.12(14) . . ? O1 Zn2 Cl3 81.20(11) . . ? N3 Zn2 Cl3 138.35(16) . . ? N4 Zn2 Cl3 91.67(16) . . ? Cl2 Zn2 Cl3 113.04(8) . . ? Zn2 Cl3 Zn1 85.12(6) . . ? C1 O1 Zn1 122.3(3) . . ? C1 O1 Zn2 126.5(3) . . ? Zn1 O1 Zn2 111.17(17) . . ? C12 N1 C11 110.3(5) . . ? C12 N1 C8 109.2(5) . . ? C11 N1 C8 109.8(5) . . ? C12 N1 Zn1 106.3(4) . . ? C11 N1 Zn1 112.8(4) . . ? C8 N1 Zn1 108.5(4) . . ? C15 N2 C14 108.9(5) . . ? C15 N2 C13 111.1(6) . . ? C14 N2 C13 107.8(5) . . ? C15 N2 Zn1 112.0(4) . . ? C14 N2 Zn1 112.9(4) . . ? C13 N2 Zn1 104.1(4) . . ? C16 N3 C9 111.0(5) . . ? C16 N3 C17 110.7(5) . . ? C9 N3 C17 108.5(5) . . ? C16 N3 Zn2 111.3(4) . . ? C9 N3 Zn2 109.8(4) . . ? C17 N3 Zn2 105.3(4) . . ? C18 N4 C19 111.2(6) . . ? C18 N4 C20 109.6(6) . . ? C19 N4 C20 108.5(6) . . ? C18 N4 Zn2 102.9(4) . . ? C19 N4 Zn2 113.7(4) . . ? C20 N4 Zn2 110.9(4) . . ? O1 C1 C2 120.6(5) . . ? O1 C1 C6 120.4(5) . . ? C2 C1 C6 118.9(5) . . ? C3 C2 C1 120.4(6) . . ? C3 C2 C8 120.8(6) . . ? C1 C2 C8 118.7(5) . . ? C2 C3 C4 121.7(6) . . ? C5 C4 C3 116.8(6) . . ? C5 C4 C7 122.2(6) . . ? C3 C4 C7 121.0(6) . . ? C6 C5 C4 122.7(6) . . ? C5 C6 C1 119.2(5) . . ? C5 C6 C9 120.6(6) . . ? C1 C6 C9 120.2(5) . . ? C2 C8 N1 114.1(5) . . ? N3 C9 C6 112.5(5) . . ? N1 C12 C13 110.0(6) . . ? N2 C13 C12 110.4(5) . . ? N3 C17 C18 110.2(6) . . ? N4 C18 C17 109.8(6) . . ? C5S O1S C2S 76.2(16) . . ? C3S C2S O1S 127(2) . . ? C2S C3S C4S 95.9(17) . . ? C5S C4S C3S 100.4(16) . . ? C4S C5S O1S 128(2) . . ? C10S O6S C7S 74.4(17) . . ? C8S C7S O6S 129(2) . . ? C8S C7S C10S 80.0(15) . . ? O6S C7S C10S 52.6(9) . . ? C7S C8S C9S 100.0(17) . . ? C10S C9S C8S 98.8(16) . . ? C9S C10S O6S 131(2) . . ? C9S C10S C7S 81.1(15) . . ? O6S C10S C7S 53.1(9) . . ? 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 O1 Zn2 Cl3 Zn1 -12.82(14) . . . . ? N3 Zn2 Cl3 Zn1 -89.1(2) . . . . ? N4 Zn2 Cl3 Zn1 -170.35(15) . . . . ? Cl2 Zn2 Cl3 Zn1 85.72(7) . . . . ? O1 Zn1 Cl3 Zn2 13.67(15) . . . . ? N2 Zn1 Cl3 Zn2 -118.68(16) . . . . ? N1 Zn1 Cl3 Zn2 -48.4(4) . . . . ? Cl1 Zn1 Cl3 Zn2 133.41(6) . . . . ? N2 Zn1 O1 C1 -120.1(5) . . . . ? N1 Zn1 O1 C1 -38.1(5) . . . . ? Cl1 Zn1 O1 C1 64.8(5) . . . . ? Cl3 Zn1 O1 C1 160.5(5) . . . . ? N2 Zn1 O1 Zn2 62.7(3) . . . . ? N1 Zn1 O1 Zn2 144.6(2) . . . . ? Cl1 Zn1 O1 Zn2 -112.48(18) . . . . ? Cl3 Zn1 O1 Zn2 -16.73(18) . . . . ? N3 Zn2 O1 C1 -19.4(5) . . . . ? N4 Zn2 O1 C1 -85.5(7) . . . . ? Cl2 Zn2 O1 C1 89.0(5) . . . . ? Cl3 Zn2 O1 C1 -159.1(5) . . . . ? N3 Zn2 O1 Zn1 157.7(3) . . . . ? N4 Zn2 O1 Zn1 91.6(5) . . . . ? Cl2 Zn2 O1 Zn1 -93.9(2) . . . . ? Cl3 Zn2 O1 Zn1 17.98(19) . . . . ? O1 Zn1 N1 C12 -129.8(4) . . . . ? N2 Zn1 N1 C12 1.6(4) . . . . ? Cl1 Zn1 N1 C12 108.4(4) . . . . ? Cl3 Zn1 N1 C12 -69.8(6) . . . . ? O1 Zn1 N1 C11 109.2(4) . . . . ? N2 Zn1 N1 C11 -119.3(4) . . . . ? Cl1 Zn1 N1 C11 -12.6(4) . . . . ? Cl3 Zn1 N1 C11 169.2(3) . . . . ? O1 Zn1 N1 C8 -12.5(4) . . . . ? N2 Zn1 N1 C8 118.9(4) . . . . ? Cl1 Zn1 N1 C8 -134.3(4) . . . . ? Cl3 Zn1 N1 C8 47.5(6) . . . . ? O1 Zn1 N2 C15 -8.5(6) . . . . ? N1 Zn1 N2 C15 -94.0(5) . . . . ? Cl1 Zn1 N2 C15 167.1(4) . . . . ? Cl3 Zn1 N2 C15 65.9(5) . . . . ? O1 Zn1 N2 C14 -131.8(4) . . . . ? N1 Zn1 N2 C14 142.7(5) . . . . ? Cl1 Zn1 N2 C14 43.8(5) . . . . ? Cl3 Zn1 N2 C14 -57.4(4) . . . . ? O1 Zn1 N2 C13 111.5(4) . . . . ? N1 Zn1 N2 C13 26.0(4) . . . . ? Cl1 Zn1 N2 C13 -72.8(4) . . . . ? Cl3 Zn1 N2 C13 -174.0(4) . . . . ? O1 Zn2 N3 C16 91.2(4) . . . . ? N4 Zn2 N3 C16 -110.3(4) . . . . ? Cl2 Zn2 N3 C16 -9.8(4) . . . . ? Cl3 Zn2 N3 C16 165.1(3) . . . . ? O1 Zn2 N3 C9 -32.1(4) . . . . ? N4 Zn2 N3 C9 126.4(4) . . . . ? Cl2 Zn2 N3 C9 -133.1(4) . . . . ? Cl3 Zn2 N3 C9 41.8(5) . . . . ? O1 Zn2 N3 C17 -148.7(4) . . . . ? N4 Zn2 N3 C17 9.7(4) . . . . ? Cl2 Zn2 N3 C17 110.2(4) . . . . ? Cl3 Zn2 N3 C17 -74.8(5) . . . . ? O1 Zn2 N4 C18 87.4(6) . . . . ? N3 Zn2 N4 C18 20.3(4) . . . . ? Cl2 Zn2 N4 C18 -87.1(4) . . . . ? Cl3 Zn2 N4 C18 158.9(4) . . . . ? O1 Zn2 N4 C19 -32.9(8) . . . . ? N3 Zn2 N4 C19 -100.0(5) . . . . ? Cl2 Zn2 N4 C19 152.6(5) . . . . ? Cl3 Zn2 N4 C19 38.6(5) . . . . ? O1 Zn2 N4 C20 -155.5(5) . . . . ? N3 Zn2 N4 C20 137.5(5) . . . . ? Cl2 Zn2 N4 C20 30.0(5) . . . . ? Cl3 Zn2 N4 C20 -84.0(5) . . . . ? Zn1 O1 C1 C2 47.0(7) . . . . ? Zn2 O1 C1 C2 -136.2(5) . . . . ? Zn1 O1 C1 C6 -136.5(5) . . . . ? Zn2 O1 C1 C6 40.3(8) . . . . ? O1 C1 C2 C3 -177.6(5) . . . . ? C6 C1 C2 C3 5.9(9) . . . . ? O1 C1 C2 C8 6.7(8) . . . . ? C6 C1 C2 C8 -169.8(5) . . . . ? C1 C2 C3 C4 -1.0(9) . . . . ? C8 C2 C3 C4 174.6(6) . . . . ? C2 C3 C4 C5 -3.4(9) . . . . ? C2 C3 C4 C7 176.8(6) . . . . ? C3 C4 C5 C6 3.0(9) . . . . ? C7 C4 C5 C6 -177.2(6) . . . . ? C4 C5 C6 C1 1.8(9) . . . . ? C4 C5 C6 C9 -178.0(6) . . . . ? O1 C1 C6 C5 177.2(5) . . . . ? C2 C1 C6 C5 -6.3(8) . . . . ? O1 C1 C6 C9 -3.0(8) . . . . ? C2 C1 C6 C9 173.5(5) . . . . ? C3 C2 C8 N1 118.1(6) . . . . ? C1 C2 C8 N1 -66.2(7) . . . . ? C12 N1 C8 C2 174.0(5) . . . . ? C11 N1 C8 C2 -65.0(7) . . . . ? Zn1 N1 C8 C2 58.6(6) . . . . ? C16 N3 C9 C6 -52.7(7) . . . . ? C17 N3 C9 C6 -174.6(5) . . . . ? Zn2 N3 C9 C6 70.7(6) . . . . ? C5 C6 C9 N3 122.0(6) . . . . ? C1 C6 C9 N3 -57.9(8) . . . . ? C11 N1 C12 C13 93.2(6) . . . . ? C8 N1 C12 C13 -146.1(5) . . . . ? Zn1 N1 C12 C13 -29.3(6) . . . . ? C15 N2 C13 C12 69.5(7) . . . . ? C14 N2 C13 C12 -171.2(6) . . . . ? Zn1 N2 C13 C12 -51.1(6) . . . . ? N1 C12 C13 N2 56.1(7) . . . . ? C16 N3 C17 C18 81.5(7) . . . . ? C9 N3 C17 C18 -156.4(6) . . . . ? Zn2 N3 C17 C18 -38.9(7) . . . . ? C19 N4 C18 C17 74.0(7) . . . . ? C20 N4 C18 C17 -166.0(6) . . . . ? Zn2 N4 C18 C17 -48.0(6) . . . . ? N3 C17 C18 N4 62.1(8) . . . . ? C5S O1S C2S C3S 32(4) . . . . ? O1S C2S C3S C4S -41(4) . . . . ? C2S C3S C4S C5S 24(4) . . . . ? C3S C4S C5S O1S -10(5) . . . . ? C2S O1S C5S C4S -9(4) . . . . ? C10S O6S C7S C8S -27(5) . . . . ? O6S C7S C8S C9S 24(6) . . . . ? C10S C7S C8S C9S 2(3) . . . . ? C7S C8S C9S C10S -3(5) . . . . ? C8S C9S C10S O6S -17(6) . . . . ? C8S C9S C10S C7S 2(3) . . . . ? C7S O6S C10S C9S 24(5) . . . . ? C8S C7S C10S C9S -3(4) . . . . ? O6S C7S C10S C9S -162(4) . . . . ? C8S C7S C10S O6S 159(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.612 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.091 #===END