data_mk373 _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H42 Cl Mg N3 O, C H2 Cl2' _chemical_formula_sum 'C30 H44 Cl3 Mg N3 O' _chemical_formula_weight 593.34 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' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.9066(5) _cell_length_b 17.5510(13) _cell_length_c 22.4279(18) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3112.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4196 _cell_measurement_theta_min 1.82 _cell_measurement_theta_max 25.0 _exptl_crystal_description 'needle' _exptl_crystal_colour 'colorless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.266 _exptl_crystal_F_000 1264 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.120 _exptl_absorpt_coefficient_mu 0.342 _shelx_estimated_absorpt_T_min 0.904 _shelx_estimated_absorpt_T_max 0.960 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.904 _exptl_absorpt_correction_T_max 0.960 _exptl_absorpt_process_details 'Sadabs, Bruker-AXS' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'ImuS micro-focus' _diffrn_measurement_device_type 'ApexDuo, Bruker-AXS' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 1.75 _diffrn_reflns_number 6450 _diffrn_reflns_av_unetI/netI 0.0628 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.816 _diffrn_reflns_theta_max 25.027 _diffrn_reflns_theta_full 25.027 _diffrn_measured_fraction_theta_max 0.980 _diffrn_measured_fraction_theta_full 0.980 _diffrn_reflns_Laue_measured_fraction_max 0.980 _diffrn_reflns_Laue_measured_fraction_full 0.980 _diffrn_reflns_point_group_measured_fraction_max 0.983 _diffrn_reflns_point_group_measured_fraction_full 0.983 _reflns_number_total 4786 _reflns_number_gt 4196 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.761 _reflns_Friedel_fraction_max 0.986 _reflns_Friedel_fraction_full 0.986 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Apex2, Bruker-AXS' _computing_cell_refinement 'Saint, Bruker-AXS' _computing_data_reduction 'Saint, Bruker-AXS' _computing_structure_solution 'SHELXT-2014 (sheldrick, 2015)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2015)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refined as a 2-component inversion twin. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0895P)^2^+5.2670P] 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 ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.05(14) _chemical_absolute_configuration ad _refine_ls_number_reflns 4786 _refine_ls_number_parameters 350 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.1718 _refine_ls_wR_factor_gt 0.1638 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.012 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.8111(2) 0.33985(11) 0.66582(8) 0.0147(4) Uani 1 1 d . . . . . Cl1 Cl 1.0122(2) 0.39584(10) 0.72889(8) 0.0315(4) Uani 1 1 d . . . . . Cl2 Cl 0.1119(2) 0.16749(11) 0.85819(8) 0.0369(5) Uani 1 1 d . . . . . Cl3 Cl -0.1985(3) 0.11004(18) 0.90475(18) 0.0956(12) Uani 1 1 d . . . . . O1 O 0.8187(6) 0.3528(2) 0.58162(17) 0.0210(10) Uani 1 1 d . . . . . N1 N 0.6403(6) 0.2741(3) 0.7221(2) 0.0168(11) Uani 1 1 d . . . . . N2 N 0.6041(7) 0.4236(3) 0.67857(19) 0.0152(11) Uani 1 1 d . . . . . N3 N 0.9140(7) 0.2244(3) 0.6626(2) 0.0192(11) Uani 1 1 d . . . . . C1 C 0.7764(8) 0.4153(3) 0.5517(2) 0.0168(13) Uani 1 1 d . . . . . C2 C 0.5538(8) 0.3295(4) 0.7617(2) 0.0174(13) Uani 1 1 d . . . . . H2 H 0.6351 0.3502 0.7918 0.021 Uiso 1 1 calc R U . . . C3 C 0.8673(8) 0.1814(3) 0.7100(2) 0.0189(13) Uani 1 1 d . . . . . C4 C 0.8185(9) 0.5085(3) 0.4738(2) 0.0193(13) Uani 1 1 d . . . . . H4 H 0.8820 0.5257 0.4405 0.023 Uiso 1 1 calc R U . . . C5 C 0.4958(9) 0.2300(4) 0.6959(2) 0.0202(13) Uani 1 1 d . . . . . H5A H 0.5325 0.1778 0.6853 0.024 Uiso 1 1 calc R U . . . H5B H 0.4534 0.2555 0.6595 0.024 Uiso 1 1 calc R U . . . C6 C 0.4157(9) 0.2836(4) 0.7927(3) 0.0232(14) Uani 1 1 d . . . . . H6A H 0.3220 0.3170 0.8059 0.028 Uiso 1 1 calc R U . . . H6B H 0.4613 0.2560 0.8277 0.028 Uiso 1 1 calc R U . . . C7 C 0.6318(8) 0.4569(4) 0.5694(2) 0.0185(13) Uani 1 1 d . . . . . C8 C 0.8702(8) 0.4411(4) 0.5019(2) 0.0181(13) Uani 1 1 d . . . . . C9 C 1.0649(8) 0.1171(4) 0.6238(3) 0.0266(15) Uani 1 1 d . . . . . H9 H 1.1341 0.0957 0.5935 0.032 Uiso 1 1 calc R U . . . C10 C 0.4795(8) 0.3942(4) 0.7244(2) 0.0178(13) Uani 1 1 d . . . . . H10 H 0.3745 0.3763 0.7040 0.021 Uiso 1 1 calc R U . . . C11 C 0.7577(9) 0.2229(4) 0.7549(2) 0.0212(14) Uani 1 1 d . . . . . H11A H 0.6926 0.1858 0.7789 0.025 Uiso 1 1 calc R U . . . H11B H 0.8296 0.2532 0.7822 0.025 Uiso 1 1 calc R U . . . C12 C 0.9186(8) 0.1070(4) 0.7164(3) 0.0246(14) Uani 1 1 d . . . . . H12 H 0.8876 0.0783 0.7506 0.030 Uiso 1 1 calc R U . . . C13 C 0.9686(9) 0.3122(4) 0.4649(3) 0.0243(15) Uani 1 1 d . . . . . H13A H 1.0681 0.2820 0.4539 0.036 Uiso 1 1 calc R U . . . H13B H 0.8882 0.3127 0.4316 0.036 Uiso 1 1 calc R U . . . H13C H 0.9146 0.2897 0.5001 0.036 Uiso 1 1 calc R U . . . C14 C 0.5199(8) 0.4260(4) 0.6179(2) 0.0166(12) Uani 1 1 d . . . . . H14A H 0.4841 0.3738 0.6069 0.020 Uiso 1 1 calc R U . . . H14B H 0.4170 0.4579 0.6205 0.020 Uiso 1 1 calc R U . . . C15 C 0.6204(10) 0.6249(4) 0.4602(3) 0.0291(16) Uani 1 1 d . . . . . C16 C 0.6509(9) 0.5021(4) 0.6986(3) 0.0238(15) Uani 1 1 d . . . . . H16A H 0.7741 0.5104 0.6942 0.029 Uiso 1 1 calc R U . . . H16B H 0.5903 0.5408 0.6747 0.029 Uiso 1 1 calc R U . . . C17 C 0.4375(9) 0.4631(4) 0.7646(3) 0.0243(15) Uani 1 1 d . . . . . H17A H 0.3422 0.4932 0.7483 0.029 Uiso 1 1 calc R U . . . H17B H 0.4101 0.4469 0.8057 0.029 Uiso 1 1 calc R U . . . C18 C 1.0239(8) 0.3953(4) 0.4794(2) 0.0210(13) Uani 1 1 d . . . . . C19 C 0.5867(9) 0.5236(4) 0.5400(3) 0.0219(14) Uani 1 1 d . . . . . H19 H 0.4897 0.5509 0.5529 0.026 Uiso 1 1 calc R U . . . C20 C 1.0104(8) 0.1920(4) 0.6206(3) 0.0201(13) Uani 1 1 d . . . . . H20 H 1.0430 0.2217 0.5872 0.024 Uiso 1 1 calc R U . . . C21 C 0.6808(9) 0.5517(4) 0.4915(2) 0.0204(13) Uani 1 1 d . . . . . C22 C 1.1003(9) 0.4302(4) 0.4224(3) 0.0271(15) Uani 1 1 d . . . . . H22A H 1.1430 0.4813 0.4312 0.041 Uiso 1 1 calc R U . . . H22B H 1.0130 0.4333 0.3915 0.041 Uiso 1 1 calc R U . . . H22C H 1.1934 0.3980 0.4084 0.041 Uiso 1 1 calc R U . . . C23 C 1.1619(8) 0.3944(4) 0.5272(3) 0.0260(15) Uani 1 1 d . . . . . H23A H 1.1157 0.3734 0.5643 0.039 Uiso 1 1 calc R U . . . H23B H 1.2017 0.4465 0.5343 0.039 Uiso 1 1 calc R U . . . H23C H 1.2566 0.3628 0.5137 0.039 Uiso 1 1 calc R U . . . C24 C 1.0157(9) 0.0750(4) 0.6722(3) 0.0285(15) Uani 1 1 d . . . . . H24 H 1.0489 0.0231 0.6752 0.034 Uiso 1 1 calc R U . . . C25 C 0.3553(9) 0.2272(4) 0.7442(3) 0.0292(16) Uani 1 1 d . . . . . H25A H 0.2451 0.2434 0.7274 0.035 Uiso 1 1 calc R U . . . H25B H 0.3437 0.1752 0.7606 0.035 Uiso 1 1 calc R U . . . C26 C 0.6158(13) 0.6911(4) 0.5039(3) 0.044(2) Uani 1 1 d . . . . . H26A H 0.5356 0.6797 0.5360 0.065 Uiso 1 1 calc R U . . . H26B H 0.5798 0.7374 0.4831 0.065 Uiso 1 1 calc R U . . . H26C H 0.7288 0.6988 0.5208 0.065 Uiso 1 1 calc R U . . . C27 C 0.4407(12) 0.6138(5) 0.4344(4) 0.047(2) Uani 1 1 d . . . . . H27A H 0.3617 0.6027 0.4670 0.071 Uiso 1 1 calc R U . . . H27B H 0.4413 0.5713 0.4062 0.071 Uiso 1 1 calc R U . . . H27C H 0.4053 0.6605 0.4139 0.071 Uiso 1 1 calc R U . . . C28 C 0.7370(14) 0.6470(5) 0.4092(4) 0.060(3) Uani 1 1 d . . . . . H28A H 0.6923 0.6924 0.3892 0.090 Uiso 1 1 calc R U . . . H28B H 0.7439 0.6049 0.3806 0.090 Uiso 1 1 calc R U . . . H28C H 0.8500 0.6581 0.4249 0.090 Uiso 1 1 calc R U . . . C29 C 0.0095(11) 0.0881(5) 0.8920(4) 0.049(2) Uani 1 1 d . . . . . H29A H 0.0172 0.0432 0.8654 0.058 Uiso 1 1 calc R U . . . H29B H 0.0659 0.0755 0.9301 0.058 Uiso 1 1 calc R U . . . C30 C 0.6005(16) 0.5071(6) 0.7623(4) 0.066(3) Uani 1 1 d . . . . . H30A H 0.5831 0.5607 0.7745 0.079 Uiso 1 1 calc R U . . . H30B H 0.6871 0.4837 0.7885 0.079 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0142(10) 0.0155(10) 0.0145(8) -0.0001(8) 0.0004(8) 0.0004(9) Cl1 0.0168(8) 0.0350(10) 0.0428(9) -0.0160(7) -0.0083(7) 0.0008(8) Cl2 0.0358(10) 0.0362(10) 0.0388(9) 0.0117(8) 0.0099(8) 0.0012(9) Cl3 0.0445(15) 0.0682(19) 0.174(3) 0.042(2) 0.0409(19) -0.0020(14) O1 0.026(2) 0.021(2) 0.0164(18) 0.0021(17) 0.0038(18) 0.007(2) N1 0.015(3) 0.019(3) 0.017(2) 0.002(2) 0.002(2) -0.002(2) N2 0.018(3) 0.015(3) 0.013(2) 0.0011(19) -0.001(2) 0.000(2) N3 0.020(3) 0.018(3) 0.020(2) 0.000(2) 0.000(2) 0.004(2) C1 0.020(3) 0.016(3) 0.015(2) -0.002(2) 0.000(2) -0.003(3) C2 0.021(3) 0.018(3) 0.013(2) -0.003(2) 0.002(2) -0.002(3) C3 0.020(3) 0.016(3) 0.020(3) -0.001(2) -0.001(2) 0.001(3) C4 0.025(3) 0.019(3) 0.014(2) 0.000(2) 0.001(3) -0.010(3) C5 0.026(3) 0.017(3) 0.018(3) -0.007(2) 0.003(3) -0.006(3) C6 0.028(4) 0.020(3) 0.021(3) -0.001(3) 0.009(3) 0.001(3) C7 0.018(3) 0.023(3) 0.014(2) 0.002(2) -0.001(2) 0.002(3) C8 0.019(3) 0.022(3) 0.013(2) -0.004(2) -0.003(2) 0.001(3) C9 0.023(3) 0.026(4) 0.030(3) -0.010(3) 0.007(3) 0.004(3) C10 0.018(3) 0.020(3) 0.015(2) -0.001(2) 0.006(3) -0.003(3) C11 0.024(3) 0.021(3) 0.019(3) 0.006(3) 0.002(3) 0.003(3) C12 0.021(3) 0.020(3) 0.033(3) 0.007(3) -0.008(3) -0.005(3) C13 0.027(4) 0.028(4) 0.018(3) -0.006(3) -0.004(3) 0.010(3) C14 0.013(3) 0.024(3) 0.013(2) 0.002(2) 0.001(2) 0.005(3) C15 0.037(4) 0.023(4) 0.028(3) 0.012(3) 0.004(3) 0.005(3) C16 0.029(4) 0.015(3) 0.028(3) -0.001(3) 0.000(3) -0.005(3) C17 0.028(4) 0.017(3) 0.028(3) -0.001(3) 0.009(3) 0.006(3) C18 0.020(3) 0.026(3) 0.018(3) -0.001(2) 0.002(2) -0.001(3) C19 0.021(3) 0.026(4) 0.019(3) 0.000(3) 0.001(3) 0.006(3) C20 0.016(3) 0.020(3) 0.024(3) -0.002(2) 0.002(3) -0.001(3) C21 0.025(3) 0.019(3) 0.018(3) 0.002(2) 0.004(3) 0.000(3) C22 0.025(4) 0.033(4) 0.023(3) 0.000(3) 0.009(3) 0.003(3) C23 0.020(3) 0.034(4) 0.023(3) -0.006(3) -0.003(3) 0.004(3) C24 0.026(4) 0.021(4) 0.038(3) -0.003(3) -0.006(3) 0.005(3) C25 0.026(4) 0.024(4) 0.038(4) -0.009(3) 0.008(3) -0.006(3) C26 0.067(6) 0.027(4) 0.036(4) 0.006(3) 0.007(4) 0.012(4) C27 0.065(6) 0.038(5) 0.039(4) 0.014(4) -0.006(4) 0.012(5) C28 0.082(7) 0.049(6) 0.048(5) 0.025(4) 0.037(5) 0.023(5) C29 0.037(4) 0.052(5) 0.057(5) 0.035(4) 0.013(4) 0.010(4) C30 0.094(9) 0.046(6) 0.058(5) -0.010(5) 0.005(6) -0.010(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 Mg1 O1 1.903(4) . ? Mg1 N1 2.179(5) . ? Mg1 N3 2.185(5) . ? Mg1 N2 2.218(5) . ? Mg1 Cl1 2.344(2) . ? Cl2 C29 1.781(8) . ? Cl3 C29 1.713(9) . ? O1 C1 1.329(7) . ? N1 C2 1.485(8) . ? N1 C11 1.486(8) . ? N1 C5 1.499(8) . ? N2 C16 1.496(8) . ? N2 C10 1.514(7) . ? N2 C14 1.516(7) . ? N3 C20 1.337(8) . ? N3 C3 1.354(8) . ? C1 C7 1.413(9) . ? C1 C8 1.415(8) . ? C2 C6 1.525(9) . ? C2 C10 1.528(8) . ? C2 H2 1.0000 . ? C3 C12 1.376(9) . ? C3 C11 1.515(9) . ? C4 C21 1.384(9) . ? C4 C8 1.402(9) . ? C4 H4 0.9500 . ? C5 C25 1.551(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C25 1.546(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C19 1.391(9) . ? C7 C14 1.503(8) . ? C8 C18 1.543(9) . ? C9 C24 1.368(9) . ? C9 C20 1.386(9) . ? C9 H9 0.9500 . ? C10 C17 1.543(8) . ? C10 H10 1.0000 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C24 1.374(10) . ? C12 H12 0.9500 . ? C13 C18 1.556(9) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C28 1.519(10) . ? C15 C26 1.521(10) . ? C15 C21 1.540(9) . ? C15 C27 1.546(12) . ? C16 C30 1.486(11) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C30 1.504(13) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C23 1.530(8) . ? C18 C22 1.539(8) . ? C19 C21 1.407(9) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24 0.9500 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? 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 Mg1 N1 131.1(2) . . ? O1 Mg1 N3 93.80(19) . . ? N1 Mg1 N3 76.0(2) . . ? O1 Mg1 N2 94.13(19) . . ? N1 Mg1 N2 79.58(19) . . ? N3 Mg1 N2 153.3(2) . . ? O1 Mg1 Cl1 121.84(18) . . ? N1 Mg1 Cl1 107.03(15) . . ? N3 Mg1 Cl1 98.99(16) . . ? N2 Mg1 Cl1 98.33(15) . . ? C1 O1 Mg1 126.3(4) . . ? C2 N1 C11 112.8(4) . . ? C2 N1 C5 102.8(5) . . ? C11 N1 C5 111.0(5) . . ? C2 N1 Mg1 106.6(4) . . ? C11 N1 Mg1 102.7(4) . . ? C5 N1 Mg1 121.3(3) . . ? C16 N2 C10 105.7(4) . . ? C16 N2 C14 110.7(4) . . ? C10 N2 C14 109.5(4) . . ? C16 N2 Mg1 117.8(4) . . ? C10 N2 Mg1 110.0(3) . . ? C14 N2 Mg1 103.1(3) . . ? C20 N3 C3 118.1(5) . . ? C20 N3 Mg1 129.0(4) . . ? C3 N3 Mg1 112.9(4) . . ? O1 C1 C7 119.2(5) . . ? O1 C1 C8 122.0(6) . . ? C7 C1 C8 118.7(5) . . ? N1 C2 C6 104.8(5) . . ? N1 C2 C10 109.7(4) . . ? C6 C2 C10 111.5(5) . . ? N1 C2 H2 110.2 . . ? C6 C2 H2 110.2 . . ? C10 C2 H2 110.2 . . ? N3 C3 C12 122.0(6) . . ? N3 C3 C11 114.2(5) . . ? C12 C3 C11 123.8(6) . . ? C21 C4 C8 124.3(5) . . ? C21 C4 H4 117.9 . . ? C8 C4 H4 117.9 . . ? N1 C5 C25 106.8(4) . . ? N1 C5 H5A 110.4 . . ? C25 C5 H5A 110.4 . . ? N1 C5 H5B 110.4 . . ? C25 C5 H5B 110.4 . . ? H5A C5 H5B 108.6 . . ? C2 C6 C25 103.8(5) . . ? C2 C6 H6A 111.0 . . ? C25 C6 H6A 111.0 . . ? C2 C6 H6B 111.0 . . ? C25 C6 H6B 111.0 . . ? H6A C6 H6B 109.0 . . ? C19 C7 C1 120.6(5) . . ? C19 C7 C14 119.7(6) . . ? C1 C7 C14 119.6(5) . . ? C4 C8 C1 118.1(6) . . ? C4 C8 C18 121.5(5) . . ? C1 C8 C18 120.4(5) . . ? C24 C9 C20 117.7(6) . . ? C24 C9 H9 121.2 . . ? C20 C9 H9 121.2 . . ? N2 C10 C2 112.0(5) . . ? N2 C10 C17 105.7(5) . . ? C2 C10 C17 110.2(5) . . ? N2 C10 H10 109.6 . . ? C2 C10 H10 109.6 . . ? C17 C10 H10 109.6 . . ? N1 C11 C3 108.6(4) . . ? N1 C11 H11A 110.0 . . ? C3 C11 H11A 110.0 . . ? N1 C11 H11B 110.0 . . ? C3 C11 H11B 110.0 . . ? H11A C11 H11B 108.4 . . ? C24 C12 C3 118.5(6) . . ? C24 C12 H12 120.7 . . ? C3 C12 H12 120.7 . . ? C18 C13 H13A 109.5 . . ? C18 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C18 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 C14 N2 113.6(5) . . ? C7 C14 H14A 108.8 . . ? N2 C14 H14A 108.8 . . ? C7 C14 H14B 108.8 . . ? N2 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? C28 C15 C26 107.7(7) . . ? C28 C15 C21 111.6(6) . . ? C26 C15 C21 110.5(6) . . ? C28 C15 C27 108.0(7) . . ? C26 C15 C27 108.3(7) . . ? C21 C15 C27 110.5(6) . . ? C30 C16 N2 106.1(6) . . ? C30 C16 H16A 110.5 . . ? N2 C16 H16A 110.5 . . ? C30 C16 H16B 110.5 . . ? N2 C16 H16B 110.5 . . ? H16A C16 H16B 108.7 . . ? C30 C17 C10 101.4(6) . . ? C30 C17 H17A 111.5 . . ? C10 C17 H17A 111.5 . . ? C30 C17 H17B 111.5 . . ? C10 C17 H17B 111.5 . . ? H17A C17 H17B 109.3 . . ? C23 C18 C22 107.8(5) . . ? C23 C18 C8 109.7(5) . . ? C22 C18 C8 112.0(5) . . ? C23 C18 C13 109.7(5) . . ? C22 C18 C13 108.1(5) . . ? C8 C18 C13 109.6(5) . . ? C7 C19 C21 121.7(6) . . ? C7 C19 H19 119.1 . . ? C21 C19 H19 119.1 . . ? N3 C20 C9 123.0(6) . . ? N3 C20 H20 118.5 . . ? C9 C20 H20 118.5 . . ? C4 C21 C19 116.4(6) . . ? C4 C21 C15 124.8(5) . . ? C19 C21 C15 118.7(6) . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C9 C24 C12 120.7(6) . . ? C9 C24 H24 119.7 . . ? C12 C24 H24 119.7 . . ? C6 C25 C5 104.4(5) . . ? C6 C25 H25A 110.9 . . ? C5 C25 H25A 110.9 . . ? C6 C25 H25B 110.9 . . ? C5 C25 H25B 110.9 . . ? H25A C25 H25B 108.9 . . ? C15 C26 H26A 109.5 . . ? C15 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C15 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C15 C27 H27A 109.5 . . ? C15 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C15 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C15 C28 H28A 109.5 . . ? C15 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C15 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Cl3 C29 Cl2 109.4(5) . . ? Cl3 C29 H29A 109.8 . . ? Cl2 C29 H29A 109.8 . . ? Cl3 C29 H29B 109.8 . . ? Cl2 C29 H29B 109.8 . . ? H29A C29 H29B 108.2 . . ? C16 C30 C17 103.4(7) . . ? C16 C30 H30A 111.1 . . ? C17 C30 H30A 111.1 . . ? C16 C30 H30B 111.1 . . ? C17 C30 H30B 111.1 . . ? H30A C30 H30B 109.0 . . ? _refine_diff_density_max 1.112 _refine_diff_density_min -0.844 _refine_diff_density_rms 0.086 _shelx_res_file ; mk373.res created by SHELXL-2014/7 TITL mo_mk373_0m_a.res in P2(1)2(1)2(1) REM Old TITL mo_mk373_0m in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.142, Rweak 0.035, Alpha 0.002, Orientation as input REM Flack x = 0.135 ( 0.043 ) from Parsons' quotients REM Formula found by SHELXT: C30 N3 O Mg Cl3 CELL 0.71073 7.9066 17.5510 22.4279 90.000 90.000 90.000 ZERR 4.000 0.0005 0.0013 0.0018 0.000 0.000 0.000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H N O MG CL UNIT 120 176 12 4 4 12 TEMP -163.00 size 0.30 0.15 0.12 L.S. 5 BOND $H twin acta LIST 4 FMAP 2 PLAN -20 omit 2 10 0 omit 3 0 7 omit 4 0 9 omit 5 0 9 omit 3 9 0 omit 4 0 10 omit 0 4 1 WGHT 0.089500 5.267000 BASF 0.05309 FVAR 0.52528 MG1 5 0.811101 0.339853 0.665816 11.00000 0.01422 0.01546 = 0.01453 -0.00010 0.00037 0.00036 CL1 6 1.012170 0.395841 0.728890 11.00000 0.01681 0.03496 = 0.04278 -0.01602 -0.00829 0.00083 CL2 6 0.111870 0.167489 0.858194 11.00000 0.03575 0.03623 = 0.03876 0.01173 0.00988 0.00117 CL3 6 -0.198527 0.110042 0.904750 11.00000 0.04447 0.06817 = 0.17419 0.04188 0.04092 -0.00199 O1 4 0.818659 0.352798 0.581623 11.00000 0.02553 0.02113 = 0.01645 0.00206 0.00381 0.00662 N1 3 0.640298 0.274060 0.722090 11.00000 0.01521 0.01853 = 0.01665 0.00177 0.00159 -0.00216 N2 3 0.604109 0.423571 0.678565 11.00000 0.01760 0.01541 = 0.01266 0.00112 -0.00077 -0.00017 N3 3 0.913988 0.224359 0.662594 11.00000 0.01955 0.01835 = 0.01969 0.00042 0.00008 0.00398 C1 1 0.776353 0.415291 0.551707 11.00000 0.01963 0.01568 = 0.01507 -0.00170 -0.00004 -0.00259 C2 1 0.553817 0.329491 0.761721 11.00000 0.02091 0.01812 = 0.01320 -0.00259 0.00157 -0.00166 AFIX 13 H2 2 0.635148 0.350213 0.791771 11.00000 -1.20000 AFIX 0 C3 1 0.867254 0.181403 0.709956 11.00000 0.02038 0.01645 = 0.01990 -0.00055 -0.00119 0.00097 C4 1 0.818457 0.508513 0.473821 11.00000 0.02529 0.01877 = 0.01374 0.00026 0.00070 -0.00975 AFIX 43 H4 2 0.882046 0.525698 0.440492 11.00000 -1.20000 AFIX 0 C5 1 0.495780 0.230032 0.695948 11.00000 0.02556 0.01677 = 0.01829 -0.00704 0.00262 -0.00551 AFIX 23 H5A 2 0.532454 0.177829 0.685341 11.00000 -1.20000 H5B 2 0.453440 0.255513 0.659506 11.00000 -1.20000 AFIX 0 C6 1 0.415684 0.283556 0.792708 11.00000 0.02848 0.02021 = 0.02085 -0.00103 0.00927 0.00086 AFIX 23 H6A 2 0.322032 0.316993 0.805892 11.00000 -1.20000 H6B 2 0.461337 0.256003 0.827701 11.00000 -1.20000 AFIX 0 C7 1 0.631786 0.456851 0.569398 11.00000 0.01819 0.02349 = 0.01368 0.00183 -0.00131 0.00202 C8 1 0.870173 0.441051 0.501926 11.00000 0.01928 0.02191 = 0.01298 -0.00364 -0.00275 0.00062 C9 1 1.064931 0.117053 0.623836 11.00000 0.02340 0.02623 = 0.03019 -0.00956 0.00662 0.00363 AFIX 43 H9 2 1.134118 0.095656 0.593522 11.00000 -1.20000 AFIX 0 C10 1 0.479535 0.394229 0.724420 11.00000 0.01828 0.02046 = 0.01472 -0.00096 0.00577 -0.00267 AFIX 13 H10 2 0.374482 0.376257 0.703959 11.00000 -1.20000 AFIX 0 C11 1 0.757736 0.222946 0.754859 11.00000 0.02375 0.02107 = 0.01870 0.00638 0.00168 0.00287 AFIX 23 H11A 2 0.692602 0.185787 0.778851 11.00000 -1.20000 H11B 2 0.829591 0.253168 0.782199 11.00000 -1.20000 AFIX 0 C12 1 0.918565 0.106963 0.716369 11.00000 0.02073 0.01981 = 0.03322 0.00716 -0.00776 -0.00457 AFIX 43 H12 2 0.887565 0.078314 0.750606 11.00000 -1.20000 AFIX 0 C13 1 0.968587 0.312215 0.464908 11.00000 0.02674 0.02849 = 0.01758 -0.00591 -0.00411 0.00977 AFIX 137 H13A 2 1.068072 0.282014 0.453921 11.00000 -1.50000 H13B 2 0.888232 0.312672 0.431641 11.00000 -1.50000 H13C 2 0.914599 0.289654 0.500056 11.00000 -1.50000 AFIX 0 C14 1 0.519901 0.425968 0.617879 11.00000 0.01326 0.02357 = 0.01303 0.00250 0.00136 0.00521 AFIX 23 H14A 2 0.484052 0.373765 0.606929 11.00000 -1.20000 H14B 2 0.416999 0.457926 0.620528 11.00000 -1.20000 AFIX 0 C15 1 0.620429 0.624896 0.460166 11.00000 0.03671 0.02297 = 0.02772 0.01181 0.00355 0.00545 C16 1 0.650908 0.502051 0.698631 11.00000 0.02850 0.01520 = 0.02771 -0.00089 0.00036 -0.00549 AFIX 23 H16A 2 0.774107 0.510428 0.694250 11.00000 -1.20000 H16B 2 0.590317 0.540823 0.674722 11.00000 -1.20000 AFIX 0 C17 1 0.437492 0.463087 0.764581 11.00000 0.02799 0.01707 = 0.02770 -0.00089 0.00915 0.00634 AFIX 23 H17A 2 0.342188 0.493177 0.748297 11.00000 -1.20000 H17B 2 0.410111 0.446881 0.805745 11.00000 -1.20000 AFIX 0 C18 1 1.023933 0.395260 0.479367 11.00000 0.01975 0.02571 = 0.01752 -0.00088 0.00157 -0.00052 C19 1 0.586667 0.523575 0.539969 11.00000 0.02097 0.02613 = 0.01866 -0.00013 0.00057 0.00564 AFIX 43 H19 2 0.489711 0.550907 0.552948 11.00000 -1.20000 AFIX 0 C20 1 1.010404 0.191989 0.620650 11.00000 0.01614 0.01987 = 0.02430 -0.00197 0.00163 -0.00058 AFIX 43 H20 2 1.042983 0.221705 0.587161 11.00000 -1.20000 AFIX 0 C21 1 0.680840 0.551677 0.491472 11.00000 0.02451 0.01909 = 0.01756 0.00197 0.00364 -0.00004 C22 1 1.100291 0.430154 0.422450 11.00000 0.02482 0.03288 = 0.02347 0.00019 0.00927 0.00282 AFIX 137 H22A 2 1.143035 0.481349 0.431235 11.00000 -1.50000 H22B 2 1.013016 0.433309 0.391521 11.00000 -1.50000 H22C 2 1.193437 0.398021 0.408354 11.00000 -1.50000 AFIX 0 C23 1 1.161867 0.394424 0.527235 11.00000 0.02046 0.03429 = 0.02332 -0.00629 -0.00257 0.00427 AFIX 137 H23A 2 1.115697 0.373430 0.564308 11.00000 -1.50000 H23B 2 1.201677 0.446527 0.534298 11.00000 -1.50000 H23C 2 1.256555 0.362781 0.513749 11.00000 -1.50000 AFIX 0 C24 1 1.015665 0.074963 0.672150 11.00000 0.02631 0.02070 = 0.03846 -0.00274 -0.00553 0.00472 AFIX 43 H24 2 1.048914 0.023091 0.675161 11.00000 -1.20000 AFIX 0 C25 1 0.355295 0.227219 0.744167 11.00000 0.02553 0.02438 = 0.03761 -0.00946 0.00791 -0.00646 AFIX 23 H25A 2 0.245138 0.243352 0.727404 11.00000 -1.20000 H25B 2 0.343664 0.175152 0.760643 11.00000 -1.20000 AFIX 0 C26 1 0.615754 0.691102 0.503929 11.00000 0.06736 0.02721 = 0.03628 0.00591 0.00699 0.01205 AFIX 137 H26A 2 0.535649 0.679656 0.536048 11.00000 -1.50000 H26B 2 0.579847 0.737443 0.483098 11.00000 -1.50000 H26C 2 0.728753 0.698850 0.520830 11.00000 -1.50000 AFIX 0 C27 1 0.440716 0.613830 0.434450 11.00000 0.06525 0.03799 = 0.03854 0.01422 -0.00632 0.01230 AFIX 137 H27A 2 0.361692 0.602728 0.466972 11.00000 -1.50000 H27B 2 0.441261 0.571285 0.406152 11.00000 -1.50000 H27C 2 0.405258 0.660461 0.413921 11.00000 -1.50000 AFIX 0 C28 1 0.736985 0.647038 0.409209 11.00000 0.08202 0.04861 = 0.04847 0.02453 0.03658 0.02302 AFIX 137 H28A 2 0.692255 0.692413 0.389213 11.00000 -1.50000 H28B 2 0.743884 0.604935 0.380611 11.00000 -1.50000 H28C 2 0.850028 0.658055 0.424920 11.00000 -1.50000 AFIX 0 C29 1 0.009474 0.088121 0.891993 11.00000 0.03674 0.05228 = 0.05680 0.03536 0.01323 0.00959 AFIX 23 H29A 2 0.017217 0.043202 0.865434 11.00000 -1.20000 H29B 2 0.065890 0.075450 0.930132 11.00000 -1.20000 AFIX 0 C30 1 0.600545 0.507075 0.762331 11.00000 0.09433 0.04640 = 0.05794 -0.00953 0.00515 -0.01049 AFIX 23 H30A 2 0.583133 0.560710 0.774542 11.00000 -1.20000 H30B 2 0.687060 0.483694 0.788474 11.00000 -1.20000 AFIX 0 HKLF 4 REM mo_mk373_0m_a.res in P2(1)2(1)2(1) REM R1 = 0.0634 for 4196 Fo > 4sig(Fo) and 0.0733 for all 4786 data REM 350 parameters refined using 0 restraints END WGHT 0.0897 5.3158 REM Highest difference peak 1.412, deepest hole -0.844, 1-sigma level 0.086 Q1 1 0.4871 0.5299 0.7278 11.00000 0.05 1.41 Q2 1 -0.1469 0.1015 0.9460 11.00000 0.05 1.33 Q3 1 -0.1629 0.0693 0.8768 11.00000 0.05 0.79 Q4 1 -0.0869 0.0358 0.8631 11.00000 0.05 0.39 Q5 1 0.0146 0.1547 0.8843 11.00000 0.05 0.37 Q6 1 0.0096 0.1410 0.8337 11.00000 0.05 0.37 Q7 1 0.0074 0.1181 0.9335 11.00000 0.05 0.33 Q8 1 0.4862 0.2983 0.7737 11.00000 0.05 0.31 Q9 1 0.5096 0.6649 0.4865 11.00000 0.05 0.30 Q10 1 0.7810 0.5210 0.7198 11.00000 0.05 0.29 Q11 1 0.8167 0.6699 0.4446 11.00000 0.05 0.28 Q12 1 1.0025 0.3344 0.7323 11.00000 0.05 0.28 Q13 1 0.8386 0.0378 0.7751 11.00000 0.05 0.28 Q14 1 0.3877 0.2338 0.7123 11.00000 0.05 0.28 Q15 1 0.5773 0.6125 0.4088 11.00000 0.05 0.28 Q16 1 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25 37.40 9.50 0 5 25 86.89 10.50 0 -5 25 91.69 12.10 -1 5 25 41.00 9.50 1 -5 25 55.49 9.40 -1 -5 25 55.89 10.30 2 -5 25 56.59 9.40 -2 5 25 64.19 10.80 -2 -5 25 45.80 10.70 0 -6 25 -0.90 6.40 0 6 25 -7.10 5.90 -1 6 25 17.80 8.20 1 -6 25 21.90 8.30 -1 -6 25 38.30 9.60 0 -7 25 99.29 12.70 0 0 26 97.39 11.80 1 0 26 1.70 6.50 -1 0 26 5.80 7.60 -2 0 26 279.27 20.90 2 0 26 266.77 17.70 0 1 26 33.40 8.20 0 -1 26 41.20 9.00 -1 1 26 255.77 19.60 1 -1 26 243.88 17.70 1 1 26 262.57 18.10 -1 -1 26 250.67 19.10 -2 1 26 87.39 12.70 2 -1 26 67.49 9.70 2 1 26 84.19 10.10 -2 -1 26 71.09 11.70 0 -2 26 61.09 11.30 0 2 26 79.09 10.90 1 -2 26 56.39 9.60 -1 2 26 51.59 10.00 1 2 26 75.69 9.90 -1 -2 26 62.29 11.20 0 -3 26 17.70 7.90 0 3 26 19.80 7.50 1 -3 26 -4.80 6.50 -1 3 26 3.70 7.00 -1 -3 26 7.30 7.80 1 3 26 4.30 6.20 0 -4 26 -0.20 7.60 0 4 26 14.40 7.30 -1 4 26 17.40 7.70 1 -4 26 8.80 7.50 -1 -4 26 6.40 8.40 1 4 26 11.50 8.10 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 82979