# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mo_dm11374_0m _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H110 Mg2 N6 O4 Si4' _chemical_formula_weight 1284.63 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _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, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.638(4) _cell_length_b 23.829(10) _cell_length_c 17.341(7) _cell_angle_alpha 90 _cell_angle_beta 101.146(7) _cell_angle_gamma 90 _cell_volume 3908(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3165 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 19.92 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.092 _exptl_crystal_F_000 1392 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.040 _exptl_absorpt_coefficient_mu 0.139 _shelx_estimated_absorpt_T_min 0.953 _shelx_estimated_absorpt_T_max 0.994 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4758 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details twinabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6976 _diffrn_reflns_av_unetI/netI 0.1138 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.471 _diffrn_reflns_theta_max 25.049 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.980 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.980 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 0.980 _reflns_number_total 6976 _reflns_number_gt 3919 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; _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 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refined as a 2-component 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^)+(0.1439P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 6976 _refine_ls_number_parameters 446 _refine_ls_number_restraints 118 _refine_ls_R_factor_all 0.1521 _refine_ls_R_factor_gt 0.0814 _refine_ls_wR_factor_ref 0.2497 _refine_ls_wR_factor_gt 0.2015 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.002 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 0.2887(2) 0.37252(7) 0.77068(9) 0.0404(5) Uani 1 1 d . . . . . N1 N 0.2834(4) 0.28809(16) 0.7353(2) 0.0343(10) Uani 1 1 d . . . . . N2 N 0.1373(5) 0.15338(19) 0.7364(3) 0.0555(13) Uani 1 1 d . . . . . N3 N 0.3287(5) 0.42979(16) 0.6946(2) 0.0441(11) Uani 1 1 d . . . . . O1 O 0.4092(4) 0.35329(14) 0.86776(19) 0.0514(10) Uani 1 1 d . . . . . O2 O 0.1253(5) 0.39931(17) 0.8201(2) 0.0644(12) Uani 1 1 d D . . . . Si1 Si 0.4952(2) 0.45558(7) 0.71214(9) 0.0585(5) Uani 1 1 d . . . . . Si2 Si 0.1983(2) 0.45195(7) 0.62046(9) 0.0562(5) Uani 1 1 d . . . . . C1 C 0.4617(5) 0.3063(2) 0.8987(3) 0.0372(12) Uani 1 1 d . . . . . C2 C 0.5404(6) 0.3043(2) 0.9784(3) 0.0425(13) Uani 1 1 d . . . . . C3 C 0.5972(6) 0.2534(2) 1.0055(3) 0.0468(14) Uani 1 1 d . . . . . H3 H 0.6471 0.2521 1.0570 0.056 Uiso 1 1 calc R U . . . C4 C 0.5863(6) 0.2039(2) 0.9626(3) 0.0461(14) Uani 1 1 d . . . . . C5 C 0.5089(6) 0.2063(2) 0.8877(3) 0.0432(13) Uani 1 1 d . . . . . H5 H 0.4978 0.1737 0.8577 0.052 Uiso 1 1 calc R U . . . C6 C 0.4459(5) 0.25566(19) 0.8546(3) 0.0352(11) Uani 1 1 d . . . . . C7 C 0.3654(6) 0.2505(2) 0.7758(3) 0.0381(12) Uani 1 1 d . . . . . H7 H 0.3726 0.2164 0.7508 0.046 Uiso 1 1 calc R U . . . C8 C 0.6545(9) 0.1503(3) 0.9982(3) 0.079(2) Uani 1 1 d . . . . . H8A H 0.6588 0.1237 0.9573 0.118 Uiso 1 1 calc R U . . . H8B H 0.5996 0.1350 1.0339 0.118 Uiso 1 1 calc R U . . . H8C H 0.7485 0.1583 1.0262 0.118 Uiso 1 1 calc R U . . . C9 C 0.5551(6) 0.3565(2) 1.0296(3) 0.0538(15) Uani 1 1 d . . . . . C10 C 0.4099(8) 0.3798(3) 1.0348(3) 0.083(2) Uani 1 1 d . . . . . H10A H 0.3597 0.3894 0.9831 0.124 Uiso 1 1 calc R U . . . H10B H 0.4211 0.4128 1.0673 0.124 Uiso 1 1 calc R U . . . H10C H 0.3575 0.3521 1.0573 0.124 Uiso 1 1 calc R U . . . C11 C 0.6411(10) 0.4005(3) 0.9961(4) 0.106(3) Uani 1 1 d . . . . . H11A H 0.7324 0.3855 0.9933 0.159 Uiso 1 1 calc R U . . . H11B H 0.6525 0.4330 1.0295 0.159 Uiso 1 1 calc R U . . . H11C H 0.5928 0.4109 0.9443 0.159 Uiso 1 1 calc R U . . . C12 C 0.6321(9) 0.3436(3) 1.1146(3) 0.092(3) Uani 1 1 d . . . . . H12A H 0.5771 0.3175 1.1383 0.139 Uiso 1 1 calc R U . . . H12B H 0.6439 0.3777 1.1446 0.139 Uiso 1 1 calc R U . . . H12C H 0.7232 0.3276 1.1136 0.139 Uiso 1 1 calc R U . . . C13 C 0.2186(6) 0.27365(19) 0.6568(3) 0.0363(12) Uani 1 1 d . . . . . C14 C 0.2910(6) 0.2841(2) 0.5962(3) 0.0473(14) Uani 1 1 d . . . . . H14 H 0.3844 0.2962 0.6085 0.057 Uiso 1 1 calc R U . . . C15 C 0.2282(8) 0.2768(3) 0.5188(3) 0.0610(17) Uani 1 1 d . . . . . H15 H 0.2785 0.2842 0.4792 0.073 Uiso 1 1 calc R U . . . C16 C 0.0909(7) 0.2586(2) 0.5003(3) 0.0585(17) Uani 1 1 d . . . . . H16 H 0.0466 0.2543 0.4480 0.070 Uiso 1 1 calc R U . . . C17 C 0.0185(6) 0.2467(2) 0.5601(3) 0.0503(14) Uani 1 1 d . . . . . H17 H -0.0746 0.2344 0.5469 0.060 Uiso 1 1 calc R U . . . C18 C 0.0800(6) 0.25241(18) 0.6392(3) 0.0369(12) Uani 1 1 d . . . . . C19 C -0.0019(5) 0.2378(2) 0.7006(3) 0.0388(12) Uani 1 1 d . . . . . C20 C -0.1138(6) 0.2715(3) 0.7095(3) 0.0567(15) Uani 1 1 d . . . . . H20 H -0.1353 0.3025 0.6769 0.068 Uiso 1 1 calc R U . . . C21 C -0.1962(7) 0.2605(3) 0.7658(4) 0.0688(18) Uani 1 1 d . . . . . H21 H -0.2708 0.2838 0.7714 0.083 Uiso 1 1 calc R U . . . C22 C -0.1632(7) 0.2142(3) 0.8122(4) 0.075(2) Uani 1 1 d . . . . . H22 H -0.2157 0.2064 0.8507 0.090 Uiso 1 1 calc R U . . . C23 C -0.0549(7) 0.1792(3) 0.8036(3) 0.0606(17) Uani 1 1 d . . . . . H23 H -0.0354 0.1478 0.8358 0.073 Uiso 1 1 calc R U . . . C24 C 0.0258(6) 0.1898(2) 0.7474(3) 0.0439(13) Uani 1 1 d . . . . . C25 C 0.1060(9) 0.1208(3) 0.6650(4) 0.090(2) Uani 1 1 d . . . . . H25A H 0.0317 0.0946 0.6684 0.135 Uiso 1 1 calc R U . . . H25B H 0.1891 0.1007 0.6582 0.135 Uiso 1 1 calc R U . . . H25C H 0.0763 0.1453 0.6210 0.135 Uiso 1 1 calc R U . . . C26 C 0.1955(8) 0.1179(3) 0.8039(4) 0.088(2) Uani 1 1 d . . . . . H26A H 0.2096 0.1399 0.8511 0.132 Uiso 1 1 calc R U . . . H26B H 0.2843 0.1025 0.7970 0.132 Uiso 1 1 calc R U . . . H26C H 0.1306 0.0879 0.8079 0.132 Uiso 1 1 calc R U . . . C27 C 0.5249(11) 0.5044(4) 0.7984(5) 0.121(3) Uani 1 1 d . . . . . H27A H 0.4818 0.5400 0.7829 0.182 Uiso 1 1 calc R U . . . H27B H 0.6246 0.5094 0.8168 0.182 Uiso 1 1 calc R U . . . H27C H 0.4836 0.4887 0.8397 0.182 Uiso 1 1 calc R U . . . C28 C 0.5513(10) 0.4915(3) 0.6280(4) 0.106(3) Uani 1 1 d . . . . . H28A H 0.5534 0.4649 0.5866 0.159 Uiso 1 1 calc R U . . . H28B H 0.6440 0.5072 0.6449 0.159 Uiso 1 1 calc R U . . . H28C H 0.4857 0.5210 0.6090 0.159 Uiso 1 1 calc R U . . . C29 C 0.6259(8) 0.3964(3) 0.7391(4) 0.100(3) Uani 1 1 d . . . . . H29A H 0.6033 0.3758 0.7826 0.149 Uiso 1 1 calc R U . . . H29B H 0.7197 0.4116 0.7535 0.149 Uiso 1 1 calc R U . . . H29C H 0.6214 0.3718 0.6949 0.149 Uiso 1 1 calc R U . . . C30 C 0.2367(9) 0.4404(3) 0.5195(3) 0.096(3) Uani 1 1 d . . . . . H30A H 0.3005 0.4689 0.5083 0.145 Uiso 1 1 calc R U . . . H30B H 0.1502 0.4423 0.4814 0.145 Uiso 1 1 calc R U . . . H30C H 0.2791 0.4041 0.5171 0.145 Uiso 1 1 calc R U . . . C31 C 0.0311(8) 0.4128(3) 0.6213(4) 0.083(2) Uani 1 1 d . . . . . H31A H 0.0450 0.3737 0.6116 0.125 Uiso 1 1 calc R U . . . H31B H -0.0428 0.4274 0.5811 0.125 Uiso 1 1 calc R U . . . H31C H 0.0049 0.4171 0.6716 0.125 Uiso 1 1 calc R U . . . C32 C 0.1613(10) 0.5289(3) 0.6289(5) 0.102(3) Uani 1 1 d . . . . . H32A H 0.1056 0.5345 0.6685 0.153 Uiso 1 1 calc R U . . . H32B H 0.1103 0.5425 0.5794 0.153 Uiso 1 1 calc R U . . . H32C H 0.2489 0.5489 0.6430 0.153 Uiso 1 1 calc R U . . . C33 C 0.071(2) 0.4540(7) 0.8225(8) 0.094(4) Uani 0.5 1 d D U P A 1 H33A H -0.0264 0.4551 0.7946 0.113 Uiso 0.5 1 calc R U P A 1 H33B H 0.1255 0.4799 0.7970 0.113 Uiso 0.5 1 calc R U P A 1 C34 C 0.079(2) 0.4716(6) 0.9081(8) 0.101(3) Uani 0.5 1 d D U P A 1 H34A H 0.1750 0.4790 0.9353 0.121 Uiso 0.5 1 calc R U P A 1 H34B H 0.0186 0.5033 0.9134 0.121 Uiso 0.5 1 calc R U P A 1 C35 C 0.0218(19) 0.4171(6) 0.9328(9) 0.086(3) Uani 0.5 1 d D U P A 1 H35A H -0.0794 0.4198 0.9302 0.103 Uiso 0.5 1 calc R U P A 1 H35B H 0.0667 0.4077 0.9862 0.103 Uiso 0.5 1 calc R U P A 1 C36 C 0.054(2) 0.3726(6) 0.8759(10) 0.081(3) Uani 0.5 1 d D U P A 1 H36A H 0.1144 0.3437 0.9043 0.098 Uiso 0.5 1 calc R U P A 1 H36B H -0.0324 0.3552 0.8489 0.098 Uiso 0.5 1 calc R U P A 1 C33' C 0.1236(19) 0.4585(6) 0.8477(10) 0.097(4) Uani 0.5 1 d D U P A 2 H33C H 0.0936 0.4848 0.8050 0.117 Uiso 0.5 1 calc R U P A 2 H33D H 0.2135 0.4702 0.8790 0.117 Uiso 0.5 1 calc R U P A 2 C34' C 0.0091(19) 0.4486(6) 0.8977(9) 0.095(3) Uani 0.5 1 d D U P A 2 H34C H 0.0360 0.4681 0.9474 0.114 Uiso 0.5 1 calc R U P A 2 H34D H -0.0799 0.4642 0.8704 0.114 Uiso 0.5 1 calc R U P A 2 C35' C -0.0112(19) 0.3867(6) 0.9135(9) 0.093(3) Uani 0.5 1 d D U P A 2 H35C H 0.0129 0.3789 0.9694 0.111 Uiso 0.5 1 calc R U P A 2 H35D H -0.1088 0.3757 0.8944 0.111 Uiso 0.5 1 calc R U P A 2 C36' C 0.086(2) 0.3552(6) 0.8705(11) 0.082(3) Uani 0.5 1 d D U P A 2 H36C H 0.1674 0.3406 0.9064 0.099 Uiso 0.5 1 calc R U P A 2 H36D H 0.0368 0.3246 0.8397 0.099 Uiso 0.5 1 calc R U P 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 Mg1 0.0465(11) 0.0382(9) 0.0349(8) 0.0016(7) 0.0039(8) 0.0013(9) N1 0.035(2) 0.039(2) 0.0290(19) 0.0035(17) 0.0064(18) 0.0001(19) N2 0.051(3) 0.055(3) 0.061(3) 0.011(2) 0.013(3) 0.002(3) N3 0.051(3) 0.038(2) 0.042(2) 0.0051(19) 0.009(2) -0.007(2) O1 0.067(3) 0.044(2) 0.0384(19) -0.0008(16) -0.0034(19) 0.005(2) O2 0.069(3) 0.072(3) 0.059(2) 0.007(2) 0.029(2) 0.013(2) Si1 0.0635(12) 0.0583(10) 0.0548(10) -0.0063(8) 0.0139(9) -0.0166(9) Si2 0.0619(12) 0.0530(10) 0.0517(9) 0.0161(8) 0.0062(8) 0.0053(9) C1 0.036(3) 0.043(3) 0.033(2) 0.002(2) 0.011(2) 0.000(2) C2 0.034(3) 0.052(3) 0.041(3) 0.000(2) 0.005(2) 0.005(3) C3 0.034(3) 0.069(4) 0.035(3) 0.001(3) 0.001(2) 0.012(3) C4 0.045(3) 0.054(3) 0.039(3) 0.003(2) 0.007(3) 0.014(3) C5 0.044(3) 0.045(3) 0.040(3) 0.001(2) 0.008(2) 0.005(3) C6 0.037(3) 0.039(3) 0.031(2) 0.002(2) 0.009(2) 0.003(2) C7 0.042(3) 0.041(3) 0.034(3) -0.001(2) 0.013(2) -0.002(2) C8 0.100(6) 0.070(4) 0.056(4) 0.005(3) -0.010(4) 0.031(4) C9 0.050(4) 0.067(4) 0.039(3) -0.010(3) -0.004(3) 0.005(3) C10 0.085(6) 0.098(5) 0.060(4) -0.029(4) 0.000(4) 0.032(4) C11 0.117(8) 0.095(6) 0.100(6) -0.028(5) 0.005(5) -0.049(6) C12 0.114(7) 0.088(5) 0.054(4) -0.029(3) -0.035(4) 0.030(5) C13 0.040(3) 0.034(3) 0.036(3) 0.001(2) 0.011(2) -0.002(2) C14 0.051(4) 0.055(3) 0.038(3) 0.005(2) 0.016(3) 0.002(3) C15 0.070(5) 0.074(4) 0.044(3) 0.000(3) 0.023(3) 0.000(4) C16 0.072(5) 0.071(4) 0.027(3) -0.003(3) -0.002(3) 0.007(4) C17 0.048(4) 0.059(4) 0.037(3) -0.002(3) -0.008(3) 0.000(3) C18 0.043(3) 0.031(3) 0.037(3) 0.000(2) 0.009(2) 0.003(2) C19 0.030(3) 0.047(3) 0.039(3) -0.011(2) 0.006(2) -0.003(3) C20 0.040(4) 0.066(4) 0.062(4) -0.004(3) 0.004(3) -0.002(3) C21 0.045(4) 0.087(5) 0.077(4) -0.019(4) 0.019(4) -0.001(4) C22 0.052(5) 0.113(6) 0.069(4) -0.020(4) 0.032(4) -0.027(4) C23 0.045(4) 0.082(4) 0.055(3) 0.014(3) 0.012(3) -0.011(4) C24 0.044(3) 0.052(3) 0.036(3) -0.002(2) 0.006(2) -0.010(3) C25 0.117(7) 0.067(4) 0.094(5) 0.002(4) 0.042(5) 0.030(5) C26 0.071(5) 0.084(5) 0.105(5) 0.045(4) 0.009(4) 0.014(4) C27 0.140(9) 0.121(7) 0.106(6) -0.060(5) 0.034(6) -0.064(6) C28 0.102(7) 0.121(7) 0.101(6) 0.006(5) 0.033(5) -0.037(6) C29 0.055(5) 0.125(7) 0.122(6) 0.003(5) 0.025(5) 0.012(5) C30 0.105(6) 0.130(7) 0.048(4) 0.019(4) -0.001(4) -0.003(6) C31 0.068(5) 0.090(5) 0.083(5) 0.027(4) -0.010(4) -0.003(4) C32 0.102(7) 0.067(5) 0.137(7) 0.036(5) 0.022(6) 0.029(5) C33 0.107(8) 0.101(6) 0.084(7) -0.015(6) 0.041(6) 0.022(6) C34 0.112(7) 0.107(6) 0.094(6) -0.021(6) 0.043(6) 0.005(6) C35 0.095(6) 0.099(6) 0.075(5) -0.012(5) 0.046(5) -0.004(6) C36 0.085(5) 0.095(6) 0.075(5) -0.012(5) 0.042(5) -0.004(5) C33' 0.112(8) 0.100(6) 0.089(7) -0.015(6) 0.043(6) 0.019(7) C34' 0.103(6) 0.106(6) 0.086(5) -0.019(5) 0.044(5) 0.004(5) C35' 0.096(6) 0.110(7) 0.081(5) -0.013(6) 0.039(5) -0.002(6) C36' 0.085(6) 0.102(6) 0.070(5) -0.009(5) 0.041(5) -0.006(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O1 1.907(4) . ? Mg1 N3 1.986(4) . ? Mg1 O2 2.036(4) . ? Mg1 N1 2.101(4) . ? Mg1 Si1 3.112(3) . ? Mg1 Si2 3.202(2) . ? N1 C7 1.305(6) . ? N1 C13 1.425(6) . ? N2 C24 1.421(7) . ? N2 C25 1.443(8) . ? N2 C26 1.466(7) . ? N3 Si1 1.690(5) . ? N3 Si2 1.699(4) . ? O1 C1 1.301(5) . ? O2 C33 1.408(14) . ? O2 C36 1.436(14) . ? O2 C36' 1.464(14) . ? O2 C33' 1.492(14) . ? Si1 C28 1.861(7) . ? Si1 C27 1.872(7) . ? Si1 C29 1.889(8) . ? Si2 C31 1.865(7) . ? Si2 C32 1.878(7) . ? Si2 C30 1.879(7) . ? C1 C6 1.421(6) . ? C1 C2 1.443(6) . ? C2 C3 1.375(7) . ? C2 C9 1.517(7) . ? C3 C4 1.388(7) . ? C3 H3 0.9300 . ? C4 C5 1.368(6) . ? C4 C8 1.513(7) . ? C5 C6 1.395(6) . ? C5 H5 0.9300 . ? C6 C7 1.441(6) . ? C7 H7 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C11 1.521(9) . ? C9 C10 1.525(9) . ? C9 C12 1.548(7) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.392(7) . ? C13 C18 1.406(7) . ? C14 C15 1.373(7) . ? C14 H14 0.9300 . ? C15 C16 1.370(9) . ? C15 H15 0.9300 . ? C16 C17 1.387(8) . ? C16 H16 0.9300 . ? C17 C18 1.392(6) . ? C17 H17 0.9300 . ? C18 C19 1.484(7) . ? C19 C20 1.377(8) . ? C19 C24 1.398(7) . ? C20 C21 1.397(8) . ? C20 H20 0.9300 . ? C21 C22 1.366(9) . ? C21 H21 0.9300 . ? C22 C23 1.368(9) . ? C22 H22 0.9300 . ? C23 C24 1.383(8) . ? C23 H23 0.9300 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C34 1.530(9) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.505(10) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.521(9) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C33' C34' 1.548(10) . ? C33' H33C 0.9700 . ? C33' H33D 0.9700 . ? C34' C35' 1.521(10) . ? C34' H34C 0.9700 . ? C34' H34D 0.9700 . ? C35' C36' 1.502(9) . ? C35' H35C 0.9700 . ? C35' H35D 0.9700 . ? C36' H36C 0.9700 . ? C36' H36D 0.9700 . ? 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 N3 126.0(2) . . ? O1 Mg1 O2 95.30(18) . . ? N3 Mg1 O2 109.20(19) . . ? O1 Mg1 N1 90.23(16) . . ? N3 Mg1 N1 117.45(17) . . ? O2 Mg1 N1 116.49(18) . . ? O1 Mg1 Si1 97.03(14) . . ? N3 Mg1 Si1 29.37(14) . . ? O2 Mg1 Si1 122.22(14) . . ? N1 Mg1 Si1 119.65(13) . . ? O1 Mg1 Si2 152.12(15) . . ? N3 Mg1 Si2 27.23(13) . . ? O2 Mg1 Si2 92.63(13) . . ? N1 Mg1 Si2 109.94(12) . . ? Si1 Mg1 Si2 56.58(6) . . ? C7 N1 C13 117.2(4) . . ? C7 N1 Mg1 121.4(3) . . ? C13 N1 Mg1 119.4(3) . . ? C24 N2 C25 113.9(5) . . ? C24 N2 C26 115.3(5) . . ? C25 N2 C26 111.0(5) . . ? Si1 N3 Si2 124.1(2) . . ? Si1 N3 Mg1 115.4(2) . . ? Si2 N3 Mg1 120.4(3) . . ? C1 O1 Mg1 133.8(3) . . ? C33 O2 C36 99.3(10) . . ? C36' O2 C33' 117.8(9) . . ? C33 O2 Mg1 128.7(9) . . ? C36 O2 Mg1 130.7(7) . . ? C36' O2 Mg1 109.8(6) . . ? C33' O2 Mg1 119.3(7) . . ? N3 Si1 C28 115.9(3) . . ? N3 Si1 C27 111.3(3) . . ? C28 Si1 C27 108.6(4) . . ? N3 Si1 C29 109.8(3) . . ? C28 Si1 C29 104.8(4) . . ? C27 Si1 C29 105.9(4) . . ? N3 Si1 Mg1 35.19(14) . . ? C28 Si1 Mg1 148.2(3) . . ? C27 Si1 Mg1 98.2(3) . . ? C29 Si1 Mg1 83.3(3) . . ? N3 Si2 C31 110.6(2) . . ? N3 Si2 C32 111.6(3) . . ? C31 Si2 C32 108.0(4) . . ? N3 Si2 C30 114.2(3) . . ? C31 Si2 C30 105.1(4) . . ? C32 Si2 C30 106.9(4) . . ? N3 Si2 Mg1 32.33(15) . . ? C31 Si2 Mg1 78.32(19) . . ? C32 Si2 Mg1 122.7(3) . . ? C30 Si2 Mg1 126.9(3) . . ? O1 C1 C6 121.1(4) . . ? O1 C1 C2 120.9(4) . . ? C6 C1 C2 118.0(4) . . ? C3 C2 C1 117.1(5) . . ? C3 C2 C9 122.4(4) . . ? C1 C2 C9 120.4(4) . . ? C2 C3 C4 125.7(5) . . ? C2 C3 H3 117.2 . . ? C4 C3 H3 117.2 . . ? C5 C4 C3 116.3(5) . . ? C5 C4 C8 122.5(5) . . ? C3 C4 C8 121.1(5) . . ? C4 C5 C6 122.7(5) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C5 C6 C1 120.1(4) . . ? C5 C6 C7 115.5(4) . . ? C1 C6 C7 124.4(4) . . ? N1 C7 C6 127.7(4) . . ? N1 C7 H7 116.1 . . ? C6 C7 H7 116.1 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C2 C9 C11 109.8(5) . . ? C2 C9 C10 110.5(5) . . ? C11 C9 C10 110.1(6) . . ? C2 C9 C12 111.6(5) . . ? C11 C9 C12 107.7(6) . . ? C10 C9 C12 107.0(5) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 119.6(5) . . ? C14 C13 N1 119.1(5) . . ? C18 C13 N1 121.2(4) . . ? C15 C14 C13 121.7(6) . . ? C15 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? C16 C15 C14 119.5(5) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C15 C16 C17 119.5(5) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C16 C17 C18 122.5(6) . . ? C16 C17 H17 118.8 . . ? C18 C17 H17 118.8 . . ? C17 C18 C13 117.1(5) . . ? C17 C18 C19 120.0(5) . . ? C13 C18 C19 122.9(4) . . ? C20 C19 C24 118.6(5) . . ? C20 C19 C18 118.6(5) . . ? C24 C19 C18 122.7(5) . . ? C19 C20 C21 122.1(6) . . ? C19 C20 H20 119.0 . . ? C21 C20 H20 119.0 . . ? C22 C21 C20 117.7(6) . . ? C22 C21 H21 121.1 . . ? C20 C21 H21 121.1 . . ? C21 C22 C23 121.6(6) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C22 C23 C24 120.8(6) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C23 C24 C19 119.2(5) . . ? C23 C24 N2 121.7(5) . . ? C19 C24 N2 119.1(5) . . ? N2 C25 H25A 109.5 . . ? N2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N2 C26 H26A 109.5 . . ? N2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si1 C27 H27A 109.5 . . ? Si1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si1 C28 H28A 109.5 . . ? Si1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si1 C29 H29A 109.5 . . ? Si1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si2 C30 H30A 109.5 . . ? Si2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si2 C31 H31A 109.5 . . ? Si2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si2 C32 H32A 109.5 . . ? Si2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O2 C33 C34 109.5(12) . . ? O2 C33 H33A 109.8 . . ? C34 C33 H33A 109.8 . . ? O2 C33 H33B 109.8 . . ? C34 C33 H33B 109.8 . . ? H33A C33 H33B 108.2 . . ? C35 C34 C33 95.0(13) . . ? C35 C34 H34A 112.7 . . ? C33 C34 H34A 112.7 . . ? C35 C34 H34B 112.7 . . ? C33 C34 H34B 112.7 . . ? H34A C34 H34B 110.2 . . ? C34 C35 C36 106.4(11) . . ? C34 C35 H35A 110.5 . . ? C36 C35 H35A 110.4 . . ? C34 C35 H35B 110.4 . . ? C36 C35 H35B 110.4 . . ? H35A C35 H35B 108.6 . . ? O2 C36 C35 108.3(11) . . ? O2 C36 H36A 110.0 . . ? C35 C36 H36A 110.0 . . ? O2 C36 H36B 110.0 . . ? C35 C36 H36B 110.0 . . ? H36A C36 H36B 108.4 . . ? O2 C33' C34' 95.0(11) . . ? O2 C33' H33C 112.7 . . ? C34' C33' H33C 112.7 . . ? O2 C33' H33D 112.7 . . ? C34' C33' H33D 112.7 . . ? H33C C33' H33D 110.2 . . ? C35' C34' C33' 112.4(13) . . ? C35' C34' H34C 109.1 . . ? C33' C34' H34C 109.1 . . ? C35' C34' H34D 109.1 . . ? C33' C34' H34D 109.1 . . ? H34C C34' H34D 107.9 . . ? C36' C35' C34' 106.2(13) . . ? C36' C35' H35C 110.5 . . ? C34' C35' H35C 110.5 . . ? C36' C35' H35D 110.5 . . ? C34' C35' H35D 110.5 . . ? H35C C35' H35D 108.7 . . ? O2 C36' C35' 101.4(10) . . ? O2 C36' H36C 111.5 . . ? C35' C36' H36C 111.5 . . ? O2 C36' H36D 111.5 . . ? C35' C36' H36D 111.5 . . ? H36C C36' H36D 109.3 . . ? _refine_diff_density_max 0.298 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.071 _shelxl_version_number 2013-4 _shelx_res_file ; TITL mo_dm11374_0m in P2(1)/c CELL 0.71073 9.6378 23.8294 17.3414 90.000 101.146 90.000 ZERR 2.00 0.0039 0.0097 0.0070 0.000 0.007 0.000 LATT 1 SYMM -x, y+1/2, -z+1/2 SFAC C H N O Mg Si UNIT 144 220 12 8 4 8 OMIT -3 50.1 L.S. 4 wpdb -1 BOND $H acta size 0.35 0.20 0.04 mpla c1 > c6 mpla c13 > c18 mpla c19 > c24 FMAP 2 simu 0.01 c33 > last PLAN 10 TEMP 23 dfix 1.48 0.02 o2 c33 o2 c33' o2 c36 o2 c36' dfix 1.53 0.01 c33 c34 c34 c35 c35 c36 c33' c34' c34' c35' c35' c36' WGHT 0.143900 BASF 0.31008 FVAR 0.59148 MG1 5 0.288744 0.372521 0.770678 11.00000 0.04651 0.03816 = 0.03487 0.00161 0.00394 0.00128 N1 3 0.283450 0.288090 0.735294 11.00000 0.03460 0.03927 = 0.02904 0.00347 0.00643 0.00008 N2 3 0.137265 0.153384 0.736378 11.00000 0.05131 0.05494 = 0.06134 0.01074 0.01335 0.00222 N3 3 0.328656 0.429786 0.694645 11.00000 0.05143 0.03833 = 0.04230 0.00512 0.00861 -0.00685 O1 4 0.409170 0.353295 0.867765 11.00000 0.06688 0.04354 = 0.03845 -0.00080 -0.00343 0.00521 O2 4 0.125303 0.399307 0.820063 11.00000 0.06870 0.07221 = 0.05872 0.00718 0.02860 0.01259 SI1 6 0.495157 0.455580 0.712144 11.00000 0.06351 0.05826 = 0.05477 -0.00634 0.01389 -0.01659 SI2 6 0.198327 0.451953 0.620456 11.00000 0.06195 0.05302 = 0.05171 0.01607 0.00616 0.00527 C1 1 0.461693 0.306292 0.898691 11.00000 0.03649 0.04343 = 0.03306 0.00189 0.01053 -0.00021 C2 1 0.540382 0.304346 0.978384 11.00000 0.03352 0.05217 = 0.04101 0.00030 0.00515 0.00485 C3 1 0.597163 0.253446 1.005470 11.00000 0.03432 0.06912 = 0.03454 0.00059 0.00051 0.01206 AFIX 43 H3 2 0.647137 0.252093 1.056992 11.00000 -1.20000 AFIX 0 C4 1 0.586344 0.203913 0.962571 11.00000 0.04518 0.05352 = 0.03898 0.00310 0.00684 0.01387 C5 1 0.508884 0.206309 0.887736 11.00000 0.04423 0.04514 = 0.04038 0.00136 0.00818 0.00544 AFIX 43 H5 2 0.497762 0.173712 0.857682 11.00000 -1.20000 AFIX 0 C6 1 0.445865 0.255656 0.854636 11.00000 0.03656 0.03867 = 0.03146 0.00203 0.00917 0.00277 C7 1 0.365352 0.250545 0.775809 11.00000 0.04183 0.04103 = 0.03373 -0.00085 0.01282 -0.00224 AFIX 43 H7 2 0.372611 0.216436 0.750831 11.00000 -1.20000 AFIX 0 C8 1 0.654520 0.150323 0.998247 11.00000 0.10014 0.06976 = 0.05577 0.00509 -0.01010 0.03103 AFIX 137 H8A 2 0.658755 0.123657 0.957271 11.00000 -1.50000 H8B 2 0.599568 0.135049 1.033892 11.00000 -1.50000 H8C 2 0.748503 0.158252 1.026221 11.00000 -1.50000 AFIX 0 C9 1 0.555137 0.356451 1.029579 11.00000 0.05038 0.06744 = 0.03875 -0.01007 -0.00373 0.00545 C10 1 0.409928 0.379834 1.034804 11.00000 0.08487 0.09822 = 0.05987 -0.02901 0.00001 0.03205 AFIX 137 H10A 2 0.359743 0.389359 0.983104 11.00000 -1.50000 H10B 2 0.421113 0.412787 1.067261 11.00000 -1.50000 H10C 2 0.357532 0.352072 1.057335 11.00000 -1.50000 AFIX 0 C11 1 0.641111 0.400519 0.996077 11.00000 0.11673 0.09456 = 0.10034 -0.02836 0.00468 -0.04930 AFIX 137 H11A 2 0.732387 0.385453 0.993279 11.00000 -1.50000 H11B 2 0.652453 0.433001 1.029454 11.00000 -1.50000 H11C 2 0.592763 0.410920 0.944350 11.00000 -1.50000 AFIX 0 C12 1 0.632125 0.343578 1.114609 11.00000 0.11429 0.08767 = 0.05448 -0.02920 -0.03514 0.03042 AFIX 137 H12A 2 0.577063 0.317479 1.138307 11.00000 -1.50000 H12B 2 0.643869 0.377685 1.144627 11.00000 -1.50000 H12C 2 0.723190 0.327585 1.113628 11.00000 -1.50000 AFIX 0 C13 1 0.218601 0.273652 0.656838 11.00000 0.03991 0.03410 = 0.03620 0.00141 0.01080 -0.00168 C14 1 0.291003 0.284055 0.596230 11.00000 0.05128 0.05529 = 0.03818 0.00521 0.01590 0.00185 AFIX 43 H14 2 0.384356 0.296230 0.608499 11.00000 -1.20000 AFIX 0 C15 1 0.228215 0.276815 0.518796 11.00000 0.06956 0.07441 = 0.04387 0.00025 0.02306 -0.00040 AFIX 43 H15 2 0.278456 0.284196 0.479219 11.00000 -1.20000 AFIX 0 C16 1 0.090941 0.258628 0.500305 11.00000 0.07189 0.07147 = 0.02750 -0.00349 -0.00160 0.00657 AFIX 43 H16 2 0.046632 0.254324 0.448033 11.00000 -1.20000 AFIX 0 C17 1 0.018536 0.246682 0.560125 11.00000 0.04775 0.05941 = 0.03730 -0.00160 -0.00770 -0.00005 AFIX 43 H17 2 -0.074606 0.234376 0.546870 11.00000 -1.20000 AFIX 0 C18 1 0.079969 0.252413 0.639218 11.00000 0.04294 0.03088 = 0.03739 0.00017 0.00895 0.00262 C19 1 -0.001865 0.237770 0.700633 11.00000 0.03030 0.04699 = 0.03861 -0.01059 0.00552 -0.00297 C20 1 -0.113847 0.271469 0.709456 11.00000 0.04037 0.06559 = 0.06156 -0.00443 0.00361 -0.00229 AFIX 43 H20 2 -0.135343 0.302543 0.676891 11.00000 -1.20000 AFIX 0 C21 1 -0.196155 0.260456 0.765764 11.00000 0.04550 0.08720 = 0.07654 -0.01914 0.01897 -0.00098 AFIX 43 H21 2 -0.270836 0.283817 0.771425 11.00000 -1.20000 AFIX 0 C22 1 -0.163232 0.214220 0.812217 11.00000 0.05196 0.11309 = 0.06908 -0.01960 0.03168 -0.02659 AFIX 43 H22 2 -0.215684 0.206387 0.850652 11.00000 -1.20000 AFIX 0 C23 1 -0.054949 0.179165 0.803554 11.00000 0.04532 0.08213 = 0.05527 0.01412 0.01228 -0.01068 AFIX 43 H23 2 -0.035408 0.147843 0.835820 11.00000 -1.20000 AFIX 0 C24 1 0.025840 0.189755 0.747357 11.00000 0.04377 0.05156 = 0.03601 -0.00178 0.00646 -0.00952 C25 1 0.105959 0.120754 0.665014 11.00000 0.11745 0.06679 = 0.09417 0.00246 0.04199 0.03039 AFIX 137 H25A 2 0.031666 0.094562 0.668350 11.00000 -1.50000 H25B 2 0.189084 0.100672 0.658178 11.00000 -1.50000 H25C 2 0.076302 0.145322 0.621043 11.00000 -1.50000 AFIX 0 C26 1 0.195473 0.117854 0.803932 11.00000 0.07112 0.08388 = 0.10542 0.04454 0.00879 0.01438 AFIX 137 H26A 2 0.209593 0.139949 0.851095 11.00000 -1.50000 H26B 2 0.284290 0.102457 0.796998 11.00000 -1.50000 H26C 2 0.130649 0.087894 0.807933 11.00000 -1.50000 AFIX 0 C27 1 0.524900 0.504367 0.798397 11.00000 0.14047 0.12081 = 0.10636 -0.06033 0.03408 -0.06355 AFIX 137 H27A 2 0.481774 0.539964 0.782860 11.00000 -1.50000 H27B 2 0.624608 0.509446 0.816846 11.00000 -1.50000 H27C 2 0.483568 0.488707 0.839712 11.00000 -1.50000 AFIX 0 C28 1 0.551343 0.491501 0.627981 11.00000 0.10170 0.12137 = 0.10089 0.00597 0.03276 -0.03711 AFIX 137 H28A 2 0.553353 0.464910 0.586625 11.00000 -1.50000 H28B 2 0.643998 0.507163 0.644924 11.00000 -1.50000 H28C 2 0.485669 0.520965 0.608968 11.00000 -1.50000 AFIX 0 C29 1 0.625949 0.396412 0.739121 11.00000 0.05462 0.12537 = 0.12222 0.00317 0.02519 0.01207 AFIX 137 H29A 2 0.603265 0.375844 0.782649 11.00000 -1.50000 H29B 2 0.719694 0.411553 0.753517 11.00000 -1.50000 H29C 2 0.621362 0.371767 0.694908 11.00000 -1.50000 AFIX 0 C30 1 0.236738 0.440400 0.519482 11.00000 0.10485 0.13005 = 0.04780 0.01868 -0.00106 -0.00318 AFIX 137 H30A 2 0.300549 0.468866 0.508343 11.00000 -1.50000 H30B 2 0.150189 0.442297 0.481364 11.00000 -1.50000 H30C 2 0.279102 0.404134 0.517144 11.00000 -1.50000 AFIX 0 C31 1 0.031050 0.412798 0.621303 11.00000 0.06750 0.09022 = 0.08260 0.02662 -0.01002 -0.00277 AFIX 137 H31A 2 0.044972 0.373735 0.611591 11.00000 -1.50000 H31B 2 -0.042778 0.427406 0.581107 11.00000 -1.50000 H31C 2 0.004862 0.417100 0.671647 11.00000 -1.50000 AFIX 0 C32 1 0.161254 0.528866 0.628877 11.00000 0.10151 0.06746 = 0.13690 0.03614 0.02237 0.02938 AFIX 137 H32A 2 0.105586 0.534506 0.668537 11.00000 -1.50000 H32B 2 0.110295 0.542523 0.579353 11.00000 -1.50000 H32C 2 0.248934 0.548879 0.643043 11.00000 -1.50000 AFIX 0 PART 1 C33 1 0.071052 0.454017 0.822500 10.50000 0.10738 0.10105 = 0.08376 -0.01540 0.04099 0.02164 AFIX 23 H33A 2 -0.026401 0.455076 0.794628 10.50000 -1.20000 H33B 2 0.125462 0.479905 0.796991 10.50000 -1.20000 AFIX 0 C34 1 0.079008 0.471579 0.908113 10.50000 0.11201 0.10664 = 0.09418 -0.02068 0.04282 0.00464 AFIX 23 H34A 2 0.174974 0.479007 0.935344 10.50000 -1.20000 H34B 2 0.018552 0.503329 0.913388 10.50000 -1.20000 AFIX 0 C35 1 0.021780 0.417077 0.932765 10.50000 0.09491 0.09910 = 0.07501 -0.01215 0.04643 -0.00449 AFIX 23 H35A 2 -0.079439 0.419815 0.930157 10.50000 -1.20000 H35B 2 0.066745 0.407717 0.986198 10.50000 -1.20000 AFIX 0 C36 1 0.054492 0.372643 0.875863 10.50000 0.08503 0.09474 = 0.07464 -0.01231 0.04159 -0.00423 AFIX 23 H36A 2 0.114433 0.343736 0.904273 10.50000 -1.20000 H36B 2 -0.032412 0.355244 0.848874 10.50000 -1.20000 AFIX 0 PART 2 C33' 1 0.123610 0.458541 0.847668 10.50000 0.11217 0.09991 = 0.08860 -0.01458 0.04264 0.01913 AFIX 23 H33C 2 0.093557 0.484825 0.804997 10.50000 -1.20000 H33D 2 0.213512 0.470182 0.878998 10.50000 -1.20000 AFIX 0 C34' 1 0.009149 0.448576 0.897663 10.50000 0.10324 0.10632 = 0.08567 -0.01931 0.04432 0.00414 AFIX 23 H34C 2 0.035986 0.468138 0.947366 10.50000 -1.20000 H34D 2 -0.079856 0.464211 0.870446 10.50000 -1.20000 AFIX 0 C35' 1 -0.011237 0.386654 0.913484 10.50000 0.09605 0.11002 = 0.08056 -0.01350 0.03940 -0.00213 AFIX 23 H35C 2 0.012903 0.378939 0.969398 10.50000 -1.20000 H35D 2 -0.108755 0.375701 0.894364 10.50000 -1.20000 AFIX 0 C36' 1 0.085568 0.355232 0.870471 10.50000 0.08541 0.10226 = 0.07029 -0.00859 0.04131 -0.00610 AFIX 23 H36C 2 0.167420 0.340634 0.906364 10.50000 -1.20000 H36D 2 0.036773 0.324615 0.839717 10.50000 -1.20000 PART 0 AFIX 0 HKLF 5 1 1 0 0 0 1 0 0 0 1 REM mo_dm11374_0m in P2(1)/c REM R1 = 0.0814 for 3919 Fo > 4sig(Fo) and 0.1521 for all 6976 data REM 446 parameters refined using 118 restraints END WGHT 0.1369 0.0000 REM Highest difference peak 0.298, deepest hole -0.373, 1-sigma level 0.071 Q1 1 0.5534 0.3424 0.9783 11.00000 0.05 0.30 Q2 1 0.2765 0.3290 0.7621 11.00000 0.05 0.29 Q3 1 -0.1477 0.2546 0.8172 11.00000 0.05 0.29 Q4 1 0.1962 0.5462 0.6970 11.00000 0.05 0.29 Q5 1 0.4877 0.5019 0.7181 11.00000 0.05 0.29 Q6 1 0.1938 0.4964 0.6264 11.00000 0.05 0.28 Q7 1 0.4070 0.3720 1.0615 11.00000 0.05 0.26 Q8 1 0.6589 0.1544 1.0465 11.00000 0.05 0.25 Q9 1 0.7098 0.4040 0.7009 11.00000 0.05 0.25 Q10 1 0.4779 0.2877 1.0557 11.00000 0.05 0.24 ; _shelx_res_checksum 47911 _shelx_hkl_file ; 1 0 0 159.393 9.47628 1 2 0 0 3663.97 196.979 1 -3 0 2 384.384 26.2791 -2 3 0 0 384.384 26.2791 1 -4 0 3 128.676 16.6078 -2 4 0 0 128.676 16.6078 1 5 0 0 22.2022 10.8406 1 -6 0 4 117.747 24.3409 -2 6 0 0 117.747 24.3409 1 -7 0 5 0.70534 14.0651 -2 7 0 0 0.70534 14.0651 1 8 0 0 -6.4072 9.68857 1 9 0 0 15.8619 9.78740 1 -10 0 7 118.746 25.2817 -2 10 0 0 118.746 25.2817 1 -11 0 8 34.7310 29.8757 -2 11 0 0 34.7310 29.8757 1 12 0 0 48.0030 22.9615 1 0 1 0 0.65163 0.11678 -2 0 1 0 0.65163 0.11678 1 1 1 0 4982.41 134.062 1 2 1 0 1656.46 63.7078 1 -3 1 2 1403.27 55.4025 -2 3 1 0 1403.27 55.4025 1 -4 1 3 631.800 37.5208 -2 4 1 0 631.800 37.5208 1 5 1 0 533.642 24.3962 1 -6 1 4 63.5312 10.8444 -2 6 1 0 63.5312 10.8444 1 -7 1 5 50.9599 8.76113 -2 7 1 0 50.9599 8.76113 1 8 1 0 4.38577 7.67092 1 9 1 0 4.78046 6.73879 1 -10 1 7 12.6270 13.9053 -2 10 1 0 12.6270 13.9053 1 -11 1 8 24.2538 20.8039 -2 11 1 0 24.2538 20.8039 1 12 1 0 -4.2214 15.4076 1 0 2 0 8381.25 263.223 -2 0 2 0 8381.25 263.223 1 1 2 0 209.636 7.14314 1 2 2 0 28.9758 4.33790 1 -3 2 2 1395.76 44.8293 -2 3 2 0 1395.76 44.8293 1 -4 2 3 45.3226 7.16862 -2 4 2 0 45.3226 7.16862 1 5 2 0 102.172 8.17763 1 -6 2 4 452.297 17.7222 -2 6 2 0 452.297 17.7222 1 -7 2 5 207.099 10.7139 -2 7 2 0 207.099 10.7139 1 8 2 0 -3.9519 7.43249 1 -9 2 6 16.6381 24.1769 -2 9 2 0 16.6381 24.1769 1 -10 2 7 14.6239 10.6722 -2 10 2 0 14.6239 10.6722 1 -11 2 8 31.9368 21.0164 -2 11 2 0 31.9368 21.0164 1 12 2 0 8.65127 15.4491 1 0 3 0 7.36072 1.73620 -2 0 3 0 7.36072 1.73620 1 1 3 0 1854.87 57.8746 1 2 3 0 3495.79 84.9712 1 -3 3 2 623.637 21.8480 -2 3 3 0 623.637 21.8480 1 -4 3 3 791.858 27.1672 -2 4 3 0 791.858 27.1672 1 5 3 0 100.212 8.29574 1 -6 3 4 6.04336 10.4426 -2 6 3 0 6.04336 10.4426 1 -7 3 5 33.4035 9.95060 -2 7 3 0 33.4035 9.95060 1 8 3 0 41.4872 7.79545 1 -9 3 6 145.486 26.2165 -2 9 3 0 145.486 26.2165 1 -10 3 7 41.9309 10.9798 -2 10 3 0 41.9309 10.9798 1 -11 3 8 42.2307 20.4051 -2 11 3 0 42.2307 20.4051 1 12 3 0 4.99952 15.5055 1 0 4 0 1647.52 51.7787 -2 0 4 0 1647.52 51.7787 1 1 4 0 2.25040 1.72419 1 2 4 0 724.895 18.5443 1 -3 4 2 2696.77 85.1782 -2 3 4 0 2696.77 85.1782 1 -4 4 3 1375.19 54.8036 -2 4 4 0 1375.19 54.8036 1 5 4 0 39.4125 7.06328 1 -6 4 4 36.8101 12.5792 -2 6 4 0 36.8101 12.5792 1 -7 4 5 167.669 13.4823 -2 7 4 0 167.669 13.4823 1 8 4 0 2.36099 7.19870 1 -9 4 6 9.54924 23.9060 -2 9 4 0 9.54924 23.9060 1 -10 4 7 30.8256 12.7013 -2 10 4 0 30.8256 12.7013 1 -11 4 8 -0.6785 19.2580 -2 11 4 0 -0.6785 19.2580 1 12 4 0 -1.4358 15.1359 1 0 5 0 -5.8987 3.34820 -2 0 5 0 -5.8987 3.34820 1 1 5 0 985.587 24.6278 1 2 5 0 128.430 5.33491 1 -3 5 2 289.022 9.99008 -2 3 5 0 289.022 9.99008 1 -4 5 3 171.231 9.87831 -2 4 5 0 171.231 9.87831 1 5 5 0 207.177 9.40711 1 -6 5 4 347.230 15.4913 -2 6 5 0 347.230 15.4913 1 -7 5 5 165.416 10.8491 -2 7 5 0 165.416 10.8491 1 8 5 0 364.406 13.6531 1 -9 5 6 -37.340 24.5724 -2 9 5 0 -37.340 24.5724 1 -10 5 7 -25.576 12.4360 -2 10 5 0 -25.576 12.4360 1 -11 5 8 -28.769 21.6121 -2 11 5 0 -28.769 21.6121 1 12 5 0 33.8417 15.9248 1 0 6 0 6492.42 202.391 -2 0 6 0 6492.42 202.391 1 1 6 0 2961.64 72.1620 1 2 6 0 358.084 12.4069 1 -3 6 2 785.622 20.4810 -2 3 6 0 785.622 20.4810 1 -4 6 3 49.0522 7.42101 -2 4 6 0 49.0522 7.42101 1 5 6 0 199.177 9.41704 1 -6 6 4 38.0785 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11.1289 -2 0 8 20 7.31285 11.1289 1 -1 8 21 62.6502 19.0621 -2 1 8 20 62.6502 19.0621 1 -2 8 21 19.9537 40.6445 -2 2 8 20 19.9537 40.6445 1 6 9 16 13.2990 18.9910 -2 -6 9 20 13.2990 18.9910 1 -5 9 20 -1.0429 10.2302 1 4 9 17 7.46981 18.6358 -2 -4 9 20 7.46981 18.6358 1 3 9 18 26.2265 19.9932 -2 -3 9 20 26.2265 19.9932 1 -2 9 20 25.5270 12.4019 1 0 9 20 63.7941 12.6675 -2 0 9 20 63.7941 12.6675 1 -1 9 21 145.588 19.6619 -2 1 9 20 145.588 19.6619 1 -2 9 21 123.183 40.3695 -2 2 9 20 123.183 40.3695 1 -6 10 20 -3.2025 12.2668 1 -5 10 20 1.79912 11.7905 1 4 10 17 27.2476 21.5845 -2 -4 10 20 27.2476 21.5845 1 3 10 18 23.4738 20.2685 -2 -3 10 20 23.4738 20.2685 1 -2 10 20 13.7984 12.3402 1 1 10 19 70.9373 17.5952 -2 -1 10 20 70.9373 17.5952 1 0 10 20 39.3413 13.1288 -2 0 10 20 39.3413 13.1288 1 -1 10 21 47.8826 19.5166 -2 1 10 20 47.8826 19.5166 1 -5 11 20 2.52096 12.2269 1 4 11 17 23.0314 21.5321 -2 -4 11 20 23.0314 21.5321 1 3 11 18 -8.5698 20.7068 -2 -3 11 20 -8.5698 20.7068 1 -2 11 20 2.59691 10.5350 1 1 11 19 87.0525 19.0456 -2 -1 11 20 87.0525 19.0456 1 0 11 20 23.7696 13.2652 -2 0 11 20 23.7696 13.2652 1 1 11 20 23.4685 12.5104 1 -5 12 20 -3.3521 15.2870 1 4 12 17 40.7825 22.8428 -2 -4 12 20 40.7825 22.8428 1 3 12 18 -6.5618 21.0161 -2 -3 12 20 -6.5618 21.0161 1 -2 12 20 11.0644 10.8025 1 1 12 19 40.4194 18.3193 -2 -1 12 20 40.4194 18.3193 1 0 12 20 62.6279 13.5391 -2 0 12 20 62.6279 13.5391 1 4 13 17 30.1680 23.1839 -2 -4 13 20 30.1680 23.1839 1 3 13 18 -0.0433 21.8089 -2 -3 13 20 -0.0433 21.8089 1 -2 13 20 13.0079 11.2925 1 1 13 19 72.3548 17.6068 -2 -1 13 20 72.3548 17.6068 1 0 13 20 36.5515 18.4451 -2 0 13 20 36.5515 18.4451 1 -3 14 20 -1.8802 10.8099 1 -2 14 20 42.8097 11.9139 1 6 0 17 -14.835 24.0057 -2 -6 0 21 -14.835 24.0057 1 -5 0 21 -2.5085 14.5167 1 4 0 18 16.5927 19.9134 -2 -4 0 21 16.5927 19.9134 1 3 0 19 6.07454 18.9624 -2 -3 0 21 6.07454 18.9624 1 -2 0 21 6.02830 13.9789 1 1 0 20 114.934 39.7947 -2 -1 0 21 114.934 39.7947 1 0 0 21 52.4913 29.0166 -2 0 0 21 52.4913 29.0166 1 -1 0 22 109.979 40.6372 -2 1 0 21 109.979 40.6372 1 6 1 17 15.3159 17.0865 -2 -6 1 21 15.3159 17.0865 1 -5 1 21 -5.0696 10.2418 1 4 1 18 29.1601 14.7852 -2 -4 1 21 29.1601 14.7852 1 3 1 19 20.6429 13.0576 -2 -3 1 21 20.6429 13.0576 1 -2 1 21 3.16156 9.98295 1 1 1 20 46.7489 27.0405 -2 -1 1 21 46.7489 27.0405 1 0 1 21 38.1281 18.0904 -2 0 1 21 38.1281 18.0904 1 -1 1 22 87.5331 38.5790 -2 1 1 21 87.5331 38.5790 1 6 2 17 7.92456 16.4597 -2 -6 2 21 7.92456 16.4597 1 -5 2 21 -0.2631 10.4527 1 4 2 18 32.2149 14.3752 -2 -4 2 21 32.2149 14.3752 1 3 2 19 -2.4067 13.5329 -2 -3 2 21 -2.4067 13.5329 1 -2 2 21 15.0744 12.2849 1 1 2 20 84.0423 25.0649 -2 -1 2 21 84.0423 25.0649 1 0 2 21 45.6150 18.9284 -2 0 2 21 45.6150 18.9284 1 -1 2 22 94.6868 37.4093 -2 1 2 21 94.6868 37.4093 1 6 3 17 -3.1004 16.9762 -2 -6 3 21 -3.1004 16.9762 1 -5 3 21 8.93955 10.6837 1 4 3 18 2.51633 14.5684 -2 -4 3 21 2.51633 14.5684 1 3 3 19 13.2596 16.4685 -2 -3 3 21 13.2596 16.4685 1 -2 3 21 -1.7578 11.8779 1 1 3 20 56.8739 19.9909 -2 -1 3 21 56.8739 19.9909 1 0 3 21 56.2597 19.8548 -2 0 3 21 56.2597 19.8548 1 -1 3 22 60.4522 39.0834 -2 1 3 21 60.4522 39.0834 1 2 3 21 64.8084 26.3878 1 6 4 17 -1.4749 16.9199 -2 -6 4 21 -1.4749 16.9199 1 -5 4 21 -9.5695 10.3621 1 4 4 18 1.52911 14.8668 -2 -4 4 21 1.52911 14.8668 1 3 4 19 13.4222 14.3493 -2 -3 4 21 13.4222 14.3493 1 -2 4 21 -5.1830 11.9550 1 1 4 20 37.7776 20.2727 -2 -1 4 21 37.7776 20.2727 1 0 4 21 14.5707 26.7238 -2 0 4 21 14.5707 26.7238 1 -1 4 22 75.6129 40.1031 -2 1 4 21 75.6129 40.1031 1 6 5 17 33.1254 36.1306 -2 -6 5 21 33.1254 36.1306 1 -5 5 21 5.78176 10.5332 1 4 5 18 -27.734 16.7051 -2 -4 5 21 -27.734 16.7051 1 3 5 19 23.3128 17.3116 -2 -3 5 21 23.3128 17.3116 1 -2 5 21 23.0205 12.2722 1 1 5 20 25.4683 19.4887 -2 -1 5 21 25.4683 19.4887 1 0 5 21 38.6534 27.3556 -2 0 5 21 38.6534 27.3556 1 -1 5 22 84.1637 41.3734 -2 1 5 21 84.1637 41.3734 1 -6 6 21 11.1828 11.0627 1 -5 6 21 -1.8371 10.4283 1 4 6 18 43.0990 14.9456 -2 -4 6 21 43.0990 14.9456 1 3 6 19 5.20963 16.6166 -2 -3 6 21 5.20963 16.6166 1 -2 6 21 14.3058 12.6883 1 1 6 20 39.7893 20.2891 -2 -1 6 21 39.7893 20.2891 1 0 6 21 59.7879 17.7065 -2 0 6 21 59.7879 17.7065 1 1 6 21 44.9332 16.2732 1 -5 7 21 2.38683 10.5646 1 4 7 18 21.6716 15.0187 -2 -4 7 21 21.6716 15.0187 1 3 7 19 18.4646 17.1842 -2 -3 7 21 18.4646 17.1842 1 -2 7 21 17.6900 12.6556 1 1 7 20 67.9013 23.8009 -2 -1 7 21 67.9013 23.8009 1 0 7 21 16.3756 15.0611 -2 0 7 21 16.3756 15.0611 1 1 7 21 54.6463 16.5222 1 -5 8 21 6.11225 10.8406 1 4 8 18 19.8147 22.1968 -2 -4 8 21 19.8147 22.1968 1 3 8 19 15.7876 17.4883 -2 -3 8 21 15.7876 17.4883 1 -2 8 21 10.8092 12.5157 1 1 8 20 75.0894 25.3777 -2 -1 8 21 75.0894 25.3777 1 0 8 21 34.9096 13.4544 -2 0 8 21 34.9096 13.4544 1 -5 9 21 5.44628 16.3979 1 4 9 18 47.5324 33.3043 -2 -4 9 21 47.5324 33.3043 1 3 9 19 20.9120 21.3460 -2 -3 9 21 20.9120 21.3460 1 -2 9 21 6.58954 12.8608 1 1 9 20 35.4382 25.5564 -2 -1 9 21 35.4382 25.5564 1 0 9 21 28.1692 13.3160 -2 0 9 21 28.1692 13.3160 1 4 10 18 7.57372 23.2303 -2 -4 10 21 7.57372 23.2303 1 3 10 19 41.5944 21.8957 -2 -3 10 21 41.5944 21.8957 1 -2 10 21 2.28610 15.8456 1 1 10 20 60.1899 25.7404 -2 -1 10 21 60.1899 25.7404 1 -3 11 21 16.3210 13.2334 1 -2 11 21 30.4380 17.0020 1 -5 0 22 28.6732 16.5453 1 4 0 19 20.4496 22.6622 -2 -4 0 22 20.4496 22.6622 1 3 0 20 39.3617 21.4253 -2 -3 0 22 39.3617 21.4253 1 -2 0 22 24.8880 24.6470 1 1 0 21 39.8136 39.8375 -2 -1 0 22 39.8136 39.8375 1 0 0 22 46.4853 30.1130 -2 0 0 22 46.4853 30.1130 1 -5 1 22 6.41056 11.1427 1 4 1 19 25.8264 16.0421 -2 -4 1 22 25.8264 16.0421 1 3 1 20 22.9384 17.4224 -2 -3 1 22 22.9384 17.4224 1 -2 1 22 12.3476 13.0258 1 1 1 21 78.0641 28.2818 -2 -1 1 22 78.0641 28.2818 1 0 1 22 61.4669 19.7413 -2 0 1 22 61.4669 19.7413 1 -5 2 22 -18.564 12.2561 1 4 2 19 26.0710 15.6616 -2 -4 2 22 26.0710 15.6616 1 3 2 20 13.7449 18.2259 -2 -3 2 22 13.7449 18.2259 1 -2 2 22 14.2185 13.1088 1 1 2 21 154.803 29.3644 -2 -1 2 22 154.803 29.3644 1 0 2 22 57.2202 30.9897 -2 0 2 22 57.2202 30.9897 1 4 3 19 56.4607 26.4977 -2 -4 3 22 56.4607 26.4977 1 3 3 20 7.91295 18.3886 -2 -3 3 22 7.91295 18.3886 1 -2 3 22 27.9707 13.6238 1 1 3 21 53.2415 28.4358 -2 -1 3 22 53.2415 28.4358 1 0 3 22 86.8299 29.4398 -2 0 3 22 86.8299 29.4398 1 4 4 19 6.16494 15.8183 -2 -4 4 22 6.16494 15.8183 1 3 4 20 20.1238 18.4559 -2 -3 4 22 20.1238 18.4559 1 -2 4 22 12.2239 12.8601 1 1 4 21 78.4646 41.8684 -2 -1 4 22 78.4646 41.8684 1 4 5 19 14.6449 14.9741 -2 -4 5 22 14.6449 14.9741 1 3 5 20 34.0461 22.6629 -2 -3 5 22 34.0461 22.6629 1 -2 5 22 4.80950 13.4392 1 1 5 21 59.0344 25.3819 -2 -1 5 22 59.0344 25.3819 1 3 6 20 61.6052 23.4071 -2 -3 6 22 61.6052 23.4071 1 -2 6 22 16.2544 13.5990 1 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 1840 _database_code_depnum_ccdc_archive 'CCDC 973421' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mo_dm11445_0m _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H88 Br2 Mg2 N6 O2 Si4' _chemical_formula_weight 1270.18 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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, -y, -z' _cell_length_a 11.442(7) _cell_length_b 13.370(8) _cell_length_c 14.072(8) _cell_angle_alpha 61.692(11) _cell_angle_beta 87.288(12) _cell_angle_gamma 70.508(11) _cell_volume 1770.7(18) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2702 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 23.79 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.191 _exptl_crystal_F_000 668 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.120 _exptl_absorpt_coefficient_mu 1.272 _shelx_estimated_absorpt_T_min 0.742 _shelx_estimated_absorpt_T_max 0.862 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6436 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12709 _diffrn_reflns_av_unetI/netI 0.0633 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.659 _diffrn_reflns_theta_max 25.998 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_point_group_measured_fraction_full 0.992 _reflns_number_total 6899 _reflns_number_gt 4143 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _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 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; ? ; _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^)+(0.1564P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 6899 _refine_ls_number_parameters 435 _refine_ls_number_restraints 249 _refine_ls_R_factor_all 0.1154 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.2421 _refine_ls_wR_factor_gt 0.1923 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.038 _refine_ls_shift/su_mean 0.003 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 Br1 Br 0.65959(6) 0.62401(5) 0.57939(5) 0.1005(4) Uani 1 1 d . . . . . Mg1 Mg 1.01477(13) 0.49433(12) 0.61069(11) 0.0397(4) Uani 1 1 d . . . . . N1 N 1.0247(3) 0.6687(3) 0.2856(3) 0.0408(8) Uani 1 1 d . . . . . N2 N 1.0916(5) 0.9772(4) 0.1276(4) 0.0774(14) Uani 1 1 d . . . . . N3 N 1.0953(4) 0.5449(4) 0.6955(3) 0.0521(9) Uani 1 1 d . . . . . O1 O 0.8973(2) 0.5927(2) 0.4718(2) 0.0422(7) Uani 1 1 d . . . . . Si1 Si 1.02400(16) 0.67743(15) 0.69902(14) 0.0688(5) Uani 1 1 d D . . . . Si2 Si 1.23993(14) 0.44868(15) 0.77039(12) 0.0661(4) Uani 1 1 d . . . . . C1 C 0.8151(4) 0.7050(4) 0.4189(3) 0.0414(9) Uani 1 1 d . . . . . C2 C 0.7000(4) 0.7441(4) 0.4517(4) 0.0515(11) Uani 1 1 d . . . . . C3 C 0.6142(4) 0.8594(4) 0.4005(4) 0.0565(12) Uani 1 1 d . . . . . H3 H 0.5376 0.8774 0.4259 0.068 Uiso 1 1 calc R U . . . C4 C 0.6418(4) 0.9506(4) 0.3096(4) 0.0532(11) Uani 1 1 d . . . . . C5 C 0.7571(4) 0.9157(4) 0.2749(4) 0.0511(11) Uani 1 1 d . . . . . H5 H 0.7780 0.9746 0.2149 0.061 Uiso 1 1 calc R U . . . C6 C 0.8425(4) 0.7970(4) 0.3255(3) 0.0420(9) Uani 1 1 d . . . . . C7 C 0.9539(4) 0.7721(4) 0.2719(3) 0.0458(10) Uani 1 1 d . . . . . H7 H 0.9746 0.8387 0.2231 0.055 Uiso 1 1 calc R U . . . C8 C 1.1239(4) 0.6640(4) 0.2188(3) 0.0442(10) Uani 1 1 d . . . . . C9 C 1.1271(5) 0.6011(5) 0.1627(4) 0.0565(12) Uani 1 1 d . . . . . H9 H 1.0641 0.5707 0.1654 0.068 Uiso 1 1 calc R U . . . C10 C 1.2240(6) 0.5838(5) 0.1027(4) 0.0692(15) Uani 1 1 d . . . . . H10 H 1.2268 0.5404 0.0664 0.083 Uiso 1 1 calc R U . . . C11 C 1.3152(6) 0.6303(6) 0.0969(5) 0.0807(18) Uani 1 1 d . . . . . H11 H 1.3796 0.6198 0.0558 0.097 Uiso 1 1 calc R U . . . C12 C 1.3117(5) 0.6920(6) 0.1514(5) 0.0696(15) Uani 1 1 d . . . . . H12 H 1.3766 0.7203 0.1483 0.083 Uiso 1 1 calc R U . . . C13 C 1.2166(4) 0.7150(4) 0.2116(4) 0.0496(11) Uani 1 1 d . . . . . C14 C 1.2224(4) 0.7782(5) 0.2740(4) 0.0531(11) Uani 1 1 d . . . . . C15 C 1.2910(5) 0.7114(6) 0.3756(4) 0.0712(15) Uani 1 1 d . . . . . H15 H 1.3314 0.6283 0.4033 0.085 Uiso 1 1 calc R U . . . C16 C 1.3029(7) 0.7624(8) 0.4390(5) 0.094(2) Uani 1 1 d . . . . . H16 H 1.3519 0.7149 0.5067 0.112 Uiso 1 1 calc R U . . . C17 C 1.2402(7) 0.8852(8) 0.3991(6) 0.092(2) Uani 1 1 d . . . . . H17 H 1.2437 0.9211 0.4410 0.111 Uiso 1 1 calc R U . . . C18 C 1.1740(7) 0.9526(6) 0.2991(5) 0.0804(17) Uani 1 1 d . . . . . H18 H 1.1330 1.0354 0.2732 0.096 Uiso 1 1 calc R U . . . C19 C 1.1638(5) 0.9047(5) 0.2330(4) 0.0633(13) Uani 1 1 d . . . . . C20 C 1.1661(9) 1.0023(7) 0.0415(6) 0.114(3) Uani 1 1 d . . . . . H20A H 1.2146 1.0463 0.0468 0.170 Uiso 1 1 calc R U . . . H20B H 1.1129 1.0503 -0.0271 0.170 Uiso 1 1 calc R U . . . H20C H 1.2212 0.9274 0.0465 0.170 Uiso 1 1 calc R U . . . C21 C 0.9914(9) 1.0928(6) 0.1106(7) 0.119(3) Uani 1 1 d . . . . . H21A H 0.9568 1.0795 0.1773 0.179 Uiso 1 1 calc R U . . . H21B H 0.9265 1.1177 0.0547 0.179 Uiso 1 1 calc R U . . . H21C H 1.0266 1.1551 0.0890 0.179 Uiso 1 1 calc R U . . . C22 C 0.5470(5) 1.0805(5) 0.2515(5) 0.0791(17) Uani 1 1 d D U . . . C23 C 0.5320(17) 1.1324(12) 0.3333(12) 0.109(4) Uani 0.5 1 d D U P A 1 H23A H 0.6059 1.0897 0.3857 0.164 Uiso 0.5 1 calc R U P A 1 H23B H 0.4608 1.1219 0.3703 0.164 Uiso 0.5 1 calc R U P A 1 H23C H 0.5202 1.2173 0.2937 0.164 Uiso 0.5 1 calc R U P A 1 C24 C 0.4239(12) 1.0791(15) 0.2123(15) 0.122(5) Uani 0.5 1 d D U P A 1 H24A H 0.4400 1.0465 0.1632 0.183 Uiso 0.5 1 calc R U P A 1 H24B H 0.3641 1.1605 0.1754 0.183 Uiso 0.5 1 calc R U P A 1 H24C H 0.3911 1.0295 0.2738 0.183 Uiso 0.5 1 calc R U P A 1 C25 C 0.5886(15) 1.1686(12) 0.1497(10) 0.090(4) Uani 0.5 1 d D U P A 1 H25A H 0.5970 1.1426 0.0960 0.136 Uiso 0.5 1 calc R U P A 1 H25B H 0.6675 1.1691 0.1693 0.136 Uiso 0.5 1 calc R U P A 1 H25C H 0.5271 1.2489 0.1205 0.136 Uiso 0.5 1 calc R U P A 1 C26 C 0.9400(19) 0.7990(11) 0.5586(10) 0.117(5) Uani 0.5 1 d D U P B 1 H26D H 0.9245 0.8776 0.5514 0.176 Uiso 0.5 1 calc R U P B 1 H26E H 0.8618 0.7911 0.5481 0.176 Uiso 0.5 1 calc R U P B 1 H26F H 0.9908 0.7902 0.5049 0.176 Uiso 0.5 1 calc R U P B 1 C27 C 0.9202(16) 0.6808(19) 0.8057(13) 0.116(6) Uani 0.5 1 d D U P B 1 H27A H 0.9289 0.7366 0.8270 0.175 Uiso 0.5 1 calc R U P B 1 H27B H 0.9440 0.6010 0.8679 0.175 Uiso 0.5 1 calc R U P B 1 H27C H 0.8348 0.7065 0.7766 0.175 Uiso 0.5 1 calc R U P B 1 C28 C 1.1393(13) 0.7493(12) 0.7041(14) 0.087(4) Uani 0.5 1 d D U P B 1 H28A H 1.1065 0.7983 0.7384 0.130 Uiso 0.5 1 calc R U P B 1 H28B H 1.1526 0.7993 0.6314 0.130 Uiso 0.5 1 calc R U P B 1 H28C H 1.2173 0.6867 0.7451 0.130 Uiso 0.5 1 calc R U P B 1 C29 C 1.3706(18) 0.464(2) 0.6855(18) 0.136(7) Uani 0.5 1 d . U P C 1 H29D H 1.4424 0.4511 0.7282 0.204 Uiso 0.5 1 calc R U P C 1 H29E H 1.3448 0.5439 0.6234 0.204 Uiso 0.5 1 calc R U P C 1 H29F H 1.3915 0.4045 0.6615 0.204 Uiso 0.5 1 calc R U P C 1 C30 C 1.2732(17) 0.2815(13) 0.8342(15) 0.101(5) Uani 0.5 1 d . U P C 1 H30A H 1.3425 0.2383 0.8913 0.151 Uiso 0.5 1 calc R U P C 1 H30B H 1.2936 0.2564 0.7800 0.151 Uiso 0.5 1 calc R U P C 1 H30C H 1.2008 0.2640 0.8640 0.151 Uiso 0.5 1 calc R U P C 1 C31 C 1.278(2) 0.4581(18) 0.8945(15) 0.126(6) Uani 0.5 1 d . U P C 1 H31D H 1.3676 0.4302 0.9115 0.189 Uiso 0.5 1 calc R U P C 1 H31E H 1.2449 0.4082 0.9551 0.189 Uiso 0.5 1 calc R U P C 1 H31F H 1.2425 0.5408 0.8797 0.189 Uiso 0.5 1 calc R U P C 1 C23' C 0.4433(14) 1.1071(12) 0.3149(13) 0.111(5) Uani 0.5 1 d D U P A 2 H23D H 0.3766 1.0849 0.3016 0.167 Uiso 0.5 1 calc R U P A 2 H23E H 0.4125 1.1923 0.2925 0.167 Uiso 0.5 1 calc R U P A 2 H23F H 0.4743 1.0612 0.3912 0.167 Uiso 0.5 1 calc R U P A 2 C24' C 0.4876(19) 1.0862(18) 0.1500(14) 0.146(6) Uani 0.5 1 d D U P A 2 H24D H 0.5444 1.0254 0.1352 0.219 Uiso 0.5 1 calc R U P A 2 H24E H 0.4719 1.1650 0.0879 0.219 Uiso 0.5 1 calc R U P A 2 H24F H 0.4104 1.0717 0.1648 0.219 Uiso 0.5 1 calc R U P A 2 C25' C 0.6068(17) 1.1737(13) 0.2097(18) 0.126(6) Uani 0.5 1 d D U P A 2 H25D H 0.6400 1.1800 0.1440 0.189 Uiso 0.5 1 calc R U P A 2 H25E H 0.6734 1.1506 0.2634 0.189 Uiso 0.5 1 calc R U P A 2 H25F H 0.5458 1.2507 0.1948 0.189 Uiso 0.5 1 calc R U P A 2 C26' C 0.8582(10) 0.7568(14) 0.6265(14) 0.104(5) Uani 0.5 1 d D U P B 2 H26A H 0.8194 0.8292 0.6321 0.156 Uiso 0.5 1 calc R U P B 2 H26B H 0.8117 0.7036 0.6595 0.156 Uiso 0.5 1 calc R U P B 2 H26C H 0.8595 0.7779 0.5512 0.156 Uiso 0.5 1 calc R U P B 2 C27' C 0.9833(15) 0.6392(14) 0.8417(8) 0.090(5) Uani 0.5 1 d D U P B 2 H27D H 0.9895 0.6989 0.8587 0.135 Uiso 0.5 1 calc R U P B 2 H27E H 1.0405 0.5605 0.8931 0.135 Uiso 0.5 1 calc R U P B 2 H27F H 0.8995 0.6387 0.8453 0.135 Uiso 0.5 1 calc R U P B 2 C28' C 1.0970(18) 0.7960(14) 0.6591(19) 0.127(7) Uani 0.5 1 d D U P B 2 H28D H 1.0794 0.8295 0.7075 0.191 Uiso 0.5 1 calc R U P B 2 H28E H 1.0632 0.8595 0.5858 0.191 Uiso 0.5 1 calc R U P B 2 H28F H 1.1859 0.7598 0.6635 0.191 Uiso 0.5 1 calc R U P B 2 C29' C 1.3482(16) 0.4008(19) 0.6834(16) 0.104(5) Uani 0.5 1 d . U P C 2 H29A H 1.4331 0.3796 0.7109 0.156 Uiso 0.5 1 calc R U P C 2 H29B H 1.3291 0.4665 0.6099 0.156 Uiso 0.5 1 calc R U P C 2 H29C H 1.3378 0.3317 0.6849 0.156 Uiso 0.5 1 calc R U P C 2 C30' C 1.2262(17) 0.3049(17) 0.8832(15) 0.112(6) Uani 0.5 1 d . U P C 2 H30D H 1.2878 0.2721 0.9443 0.168 Uiso 0.5 1 calc R U P C 2 H30E H 1.2396 0.2470 0.8582 0.168 Uiso 0.5 1 calc R U P C 2 H30F H 1.1442 0.3221 0.9048 0.168 Uiso 0.5 1 calc R U P C 2 C31' C 1.3241(17) 0.513(2) 0.8245(19) 0.121(5) Uani 0.5 1 d . U P C 2 H31A H 1.3928 0.4483 0.8784 0.182 Uiso 0.5 1 calc R U P C 2 H31B H 1.2675 0.5554 0.8569 0.182 Uiso 0.5 1 calc R U P C 2 H31C H 1.3552 0.5682 0.7660 0.182 Uiso 0.5 1 calc R U P C 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 Br1 0.0930(5) 0.0537(4) 0.0866(5) -0.0035(3) 0.0507(4) 0.0010(3) Mg1 0.0430(8) 0.0368(7) 0.0359(7) -0.0188(6) 0.0023(6) -0.0079(6) N1 0.0388(18) 0.0450(19) 0.0356(18) -0.0203(15) 0.0054(14) -0.0103(15) N2 0.102(4) 0.052(3) 0.067(3) -0.020(2) -0.005(3) -0.027(3) N3 0.058(2) 0.057(2) 0.053(2) -0.0356(19) 0.0042(18) -0.0199(19) O1 0.0394(15) 0.0358(14) 0.0395(15) -0.0174(12) -0.0012(12) -0.0001(12) Si1 0.0782(10) 0.0667(9) 0.0787(10) -0.0501(9) 0.0033(8) -0.0221(8) Si2 0.0631(9) 0.0771(10) 0.0608(9) -0.0381(8) -0.0055(7) -0.0192(8) C1 0.040(2) 0.041(2) 0.036(2) -0.0182(18) -0.0006(17) -0.0059(18) C2 0.050(3) 0.044(2) 0.046(3) -0.017(2) 0.010(2) -0.006(2) C3 0.047(3) 0.052(3) 0.049(3) -0.019(2) 0.014(2) -0.001(2) C4 0.044(2) 0.047(3) 0.051(3) -0.019(2) 0.005(2) -0.003(2) C5 0.050(3) 0.039(2) 0.050(3) -0.015(2) 0.009(2) -0.011(2) C6 0.039(2) 0.037(2) 0.045(2) -0.0195(19) 0.0045(18) -0.0094(18) C7 0.042(2) 0.044(2) 0.043(2) -0.0174(19) 0.0053(18) -0.011(2) C8 0.042(2) 0.040(2) 0.036(2) -0.0140(18) 0.0035(17) -0.0048(18) C9 0.057(3) 0.059(3) 0.056(3) -0.034(2) 0.009(2) -0.014(2) C10 0.079(4) 0.076(4) 0.062(3) -0.045(3) 0.025(3) -0.022(3) C11 0.072(4) 0.099(5) 0.073(4) -0.049(4) 0.034(3) -0.026(4) C12 0.052(3) 0.086(4) 0.070(4) -0.039(3) 0.016(3) -0.022(3) C13 0.038(2) 0.058(3) 0.042(2) -0.019(2) 0.0069(18) -0.013(2) C14 0.044(2) 0.064(3) 0.053(3) -0.027(2) 0.010(2) -0.024(2) C15 0.066(3) 0.077(4) 0.059(3) -0.026(3) -0.004(3) -0.022(3) C16 0.090(5) 0.125(6) 0.061(4) -0.036(4) -0.003(3) -0.047(5) C17 0.121(6) 0.107(6) 0.085(5) -0.056(4) 0.022(4) -0.070(5) C18 0.115(5) 0.072(4) 0.073(4) -0.037(3) 0.014(4) -0.052(4) C19 0.074(3) 0.064(3) 0.062(3) -0.028(3) 0.012(3) -0.040(3) C20 0.159(8) 0.088(5) 0.068(5) -0.017(4) 0.011(5) -0.046(5) C21 0.152(7) 0.054(4) 0.126(7) -0.030(4) -0.030(6) -0.021(4) C22 0.063(3) 0.053(3) 0.077(3) -0.013(2) 0.015(3) -0.001(2) C23 0.125(9) 0.051(6) 0.107(8) -0.039(5) 0.013(7) 0.021(6) C24 0.052(6) 0.102(8) 0.111(8) 0.009(7) -0.008(6) -0.002(6) C25 0.087(7) 0.056(6) 0.072(7) -0.010(5) 0.018(6) 0.007(5) C26 0.124(11) 0.077(8) 0.150(11) -0.070(8) -0.029(9) -0.005(7) C27 0.090(11) 0.110(11) 0.174(12) -0.089(9) 0.062(9) -0.040(9) C28 0.127(10) 0.046(7) 0.090(10) -0.033(7) 0.009(7) -0.034(7) C29 0.076(9) 0.136(13) 0.115(10) -0.018(10) 0.002(8) -0.008(9) C30 0.105(11) 0.066(7) 0.119(11) -0.047(7) -0.038(8) -0.006(7) C31 0.150(12) 0.117(11) 0.088(10) -0.055(8) -0.041(8) -0.006(9) C23' 0.095(8) 0.054(6) 0.118(8) -0.023(6) 0.033(7) 0.019(6) C24' 0.115(9) 0.112(8) 0.113(9) -0.013(7) -0.030(8) 0.015(8) C25' 0.111(8) 0.049(6) 0.151(10) -0.019(7) 0.010(9) 0.006(6) C26' 0.100(9) 0.088(8) 0.122(10) -0.075(8) -0.024(7) 0.010(7) C27' 0.096(11) 0.096(9) 0.125(10) -0.093(8) 0.035(8) -0.031(8) C28' 0.167(13) 0.069(10) 0.131(13) -0.046(9) 0.059(10) -0.035(9) C29' 0.073(8) 0.137(12) 0.105(9) -0.073(9) -0.001(7) -0.017(8) C30' 0.088(10) 0.108(10) 0.094(10) -0.021(8) -0.024(8) -0.020(8) C31' 0.111(9) 0.143(10) 0.144(10) -0.098(8) -0.018(8) -0.037(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 Br1 C2 1.924(5) . ? Mg1 O1 1.997(3) . ? Mg1 N3 2.004(4) . ? Mg1 O1 2.026(3) 2_766 ? Mg1 N1 2.160(4) 2_766 ? Mg1 Mg1 3.076(3) 2_766 ? Mg1 Si2 3.203(2) . ? Mg1 Si1 3.259(2) . ? N1 C7 1.272(5) . ? N1 C8 1.444(5) . ? N1 Mg1 2.160(4) 2_766 ? N2 C20 1.419(9) . ? N2 C19 1.428(7) . ? N2 C21 1.501(9) . ? N3 Si1 1.709(4) . ? N3 Si2 1.721(4) . ? O1 C1 1.325(5) . ? O1 Mg1 2.026(3) 2_766 ? Si1 C28' 1.877(8) . ? Si1 C27 1.877(8) . ? Si1 C26 1.887(8) . ? Si1 C26' 1.892(8) . ? Si1 C28 1.895(8) . ? Si1 C27' 1.898(8) . ? Si2 C29 1.87(2) . ? Si2 C31' 1.868(15) . ? Si2 C30 1.873(15) . ? Si2 C29' 1.874(18) . ? Si2 C31 1.891(15) . ? Si2 C30' 1.877(19) . ? C1 C2 1.391(6) . ? C1 C6 1.423(6) . ? C2 C3 1.365(6) . ? C3 C4 1.401(7) . ? C3 H3 0.9300 . ? C4 C5 1.393(6) . ? C4 C22 1.530(7) . ? C5 C6 1.393(6) . ? C5 H5 0.9300 . ? C6 C7 1.473(6) . ? C7 H7 0.9300 . ? C8 C9 1.391(6) . ? C8 C13 1.418(6) . ? C9 C10 1.385(7) . ? C9 H9 0.9300 . ? C10 C11 1.363(9) . ? C10 H10 0.9300 . ? C11 C12 1.359(8) . ? C11 H11 0.9300 . ? C12 C13 1.390(7) . ? C12 H12 0.9300 . ? C13 C14 1.494(7) . ? C14 C15 1.374(7) . ? C14 C19 1.414(7) . ? C15 C16 1.389(9) . ? C15 H15 0.9300 . ? C16 C17 1.379(10) . ? C16 H16 0.9300 . ? C17 C18 1.344(9) . ? C17 H17 0.9300 . ? C18 C19 1.384(8) . ? C18 H18 0.9300 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C25' 1.484(15) . ? C22 C23' 1.501(12) . ? C22 C25 1.540(13) . ? C22 C24 1.546(13) . ? C22 C24' 1.569(15) . ? C22 C23 1.581(13) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26D 0.9600 . ? C26 H26E 0.9600 . ? C26 H26F 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29D 0.9600 . ? C29 H29E 0.9600 . ? C29 H29F 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31D 0.9600 . ? C31 H31E 0.9600 . ? C31 H31F 0.9600 . ? C23' H23D 0.9600 . ? C23' H23E 0.9600 . ? C23' H23F 0.9600 . ? C24' H24D 0.9600 . ? C24' H24E 0.9600 . ? C24' H24F 0.9600 . ? C25' H25D 0.9600 . ? C25' H25E 0.9600 . ? C25' H25F 0.9600 . ? C26' H26A 0.9600 . ? C26' H26B 0.9600 . ? C26' H26C 0.9600 . ? C27' H27D 0.9600 . ? C27' H27E 0.9600 . ? C27' H27F 0.9600 . ? C28' H28D 0.9600 . ? C28' H28E 0.9600 . ? C28' H28F 0.9600 . ? C29' H29A 0.9600 . ? C29' H29B 0.9600 . ? C29' H29C 0.9600 . ? C30' H30D 0.9600 . ? C30' H30E 0.9600 . ? C30' H30F 0.9600 . ? C31' H31A 0.9600 . ? C31' H31B 0.9600 . ? C31' H31C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mg1 N3 130.95(16) . . ? O1 Mg1 O1 80.27(13) . 2_766 ? N3 Mg1 O1 126.26(16) . 2_766 ? O1 Mg1 N1 109.70(14) . 2_766 ? N3 Mg1 N1 112.41(16) . 2_766 ? O1 Mg1 N1 85.78(14) 2_766 2_766 ? O1 Mg1 Mg1 40.49(8) . 2_766 ? N3 Mg1 Mg1 144.60(15) . 2_766 ? O1 Mg1 Mg1 39.78(8) 2_766 2_766 ? N1 Mg1 Mg1 99.81(11) 2_766 2_766 ? O1 Mg1 Si2 152.38(11) . . ? N3 Mg1 Si2 28.22(12) . . ? O1 Mg1 Si2 102.92(10) 2_766 . ? N1 Mg1 Si2 97.91(10) 2_766 . ? Mg1 Mg1 Si2 136.26(8) 2_766 . ? O1 Mg1 Si1 107.75(10) . . ? N3 Mg1 Si1 26.25(12) . . ? O1 Mg1 Si1 144.66(11) 2_766 . ? N1 Mg1 Si1 121.02(11) 2_766 . ? Mg1 Mg1 Si1 137.34(8) 2_766 . ? Si2 Mg1 Si1 54.47(5) . . ? C7 N1 C8 118.3(4) . . ? C7 N1 Mg1 121.7(3) . 2_766 ? C8 N1 Mg1 119.5(3) . 2_766 ? C20 N2 C19 113.2(6) . . ? C20 N2 C21 110.0(6) . . ? C19 N2 C21 114.7(5) . . ? Si1 N3 Si2 119.1(2) . . ? Si1 N3 Mg1 122.5(2) . . ? Si2 N3 Mg1 118.4(2) . . ? C1 O1 Mg1 135.5(2) . . ? C1 O1 Mg1 120.4(2) . 2_766 ? Mg1 O1 Mg1 99.73(13) . 2_766 ? N3 Si1 C28' 123.1(7) . . ? N3 Si1 C27 120.1(7) . . ? N3 Si1 C26 108.2(5) . . ? C27 Si1 C26 110.7(9) . . ? N3 Si1 C26' 111.2(4) . . ? C28' Si1 C26' 107.7(9) . . ? N3 Si1 C28 112.3(5) . . ? C27 Si1 C28 106.4(9) . . ? C26 Si1 C28 96.6(8) . . ? N3 Si1 C27' 108.6(5) . . ? C28' Si1 C27' 106.0(9) . . ? C26' Si1 C27' 97.2(8) . . ? N3 Si1 Mg1 31.24(13) . . ? C28' Si1 Mg1 135.2(7) . . ? C27 Si1 Mg1 115.0(7) . . ? C26 Si1 Mg1 83.4(4) . . ? C26' Si1 Mg1 80.1(4) . . ? C28 Si1 Mg1 135.7(6) . . ? C27' Si1 Mg1 117.0(5) . . ? N3 Si2 C29 112.5(6) . . ? N3 Si2 C31' 116.3(6) . . ? N3 Si2 C30 117.3(5) . . ? C29 Si2 C30 100.7(10) . . ? N3 Si2 C29' 109.8(6) . . ? C31' Si2 C29' 104.6(9) . . ? N3 Si2 C31 116.3(6) . . ? C29 Si2 C31 108.3(11) . . ? C30 Si2 C31 99.9(8) . . ? N3 Si2 C30' 109.5(6) . . ? C31' Si2 C30' 110.7(9) . . ? C29' Si2 C30' 105.3(9) . . ? N3 Si2 Mg1 33.41(12) . . ? C29 Si2 Mg1 104.4(7) . . ? C31' Si2 Mg1 148.5(6) . . ? C30 Si2 Mg1 88.8(5) . . ? C29' Si2 Mg1 87.0(5) . . ? C31 Si2 Mg1 143.8(7) . . ? C30' Si2 Mg1 93.7(5) . . ? O1 C1 C2 123.8(4) . . ? O1 C1 C6 121.3(4) . . ? C2 C1 C6 114.8(4) . . ? C3 C2 C1 125.4(4) . . ? C3 C2 Br1 118.0(3) . . ? C1 C2 Br1 116.6(3) . . ? C2 C3 C4 119.9(4) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 116.5(4) . . ? C5 C4 C22 122.8(4) . . ? C3 C4 C22 120.6(4) . . ? C4 C5 C6 123.2(4) . . ? C4 C5 H5 118.4 . . ? C6 C5 H5 118.4 . . ? C5 C6 C1 120.1(4) . . ? C5 C6 C7 116.5(4) . . ? C1 C6 C7 123.2(4) . . ? N1 C7 C6 126.6(4) . . ? N1 C7 H7 116.7 . . ? C6 C7 H7 116.7 . . ? C9 C8 C13 120.4(4) . . ? C9 C8 N1 115.8(4) . . ? C13 C8 N1 123.8(4) . . ? C10 C9 C8 120.2(5) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C11 C10 C9 120.0(5) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C12 C11 C10 119.8(5) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 123.6(6) . . ? C11 C12 H12 118.2 . . ? C13 C12 H12 118.2 . . ? C12 C13 C8 115.9(5) . . ? C12 C13 C14 120.6(4) . . ? C8 C13 C14 123.2(4) . . ? C15 C14 C19 117.4(5) . . ? C15 C14 C13 119.0(5) . . ? C19 C14 C13 123.6(4) . . ? C14 C15 C16 123.0(6) . . ? C14 C15 H15 118.5 . . ? C16 C15 H15 118.5 . . ? C17 C16 C15 118.4(6) . . ? C17 C16 H16 120.8 . . ? C15 C16 H16 120.8 . . ? C18 C17 C16 119.6(6) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 123.2(6) . . ? C17 C18 H18 118.4 . . ? C19 C18 H18 118.4 . . ? C18 C19 C14 118.4(5) . . ? C18 C19 N2 122.5(5) . . ? C14 C19 N2 119.1(4) . . ? N2 C20 H20A 109.5 . . ? N2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N2 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C25' C22 C23' 111.5(11) . . ? C25' C22 C4 112.9(8) . . ? C23' C22 C4 114.6(7) . . ? C4 C22 C25 114.3(6) . . ? C4 C22 C24 109.1(8) . . ? C25 C22 C24 106.4(10) . . ? C25' C22 C24' 107.2(13) . . ? C23' C22 C24' 107.6(12) . . ? C4 C22 C24' 102.2(8) . . ? C4 C22 C23 107.5(6) . . ? C25 C22 C23 105.8(10) . . ? C24 C22 C23 114.1(12) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si1 C26 H26D 109.5 . . ? Si1 C26 H26E 109.5 . . ? H26D C26 H26E 109.5 . . ? Si1 C26 H26F 109.5 . . ? H26D C26 H26F 109.5 . . ? H26E C26 H26F 109.5 . . ? Si1 C27 H27A 109.5 . . ? Si1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si1 C28 H28A 109.5 . . ? Si1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si2 C29 H29D 109.5 . . ? Si2 C29 H29E 109.5 . . ? H29D C29 H29E 109.5 . . ? Si2 C29 H29F 109.5 . . ? H29D C29 H29F 109.5 . . ? H29E C29 H29F 109.5 . . ? Si2 C30 H30A 109.5 . . ? Si2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si2 C31 H31D 109.5 . . ? Si2 C31 H31E 109.5 . . ? H31D C31 H31E 109.5 . . ? Si2 C31 H31F 109.5 . . ? H31D C31 H31F 109.5 . . ? H31E C31 H31F 109.5 . . ? C22 C23' H23D 109.5 . . ? C22 C23' H23E 109.5 . . ? H23D C23' H23E 109.5 . . ? C22 C23' H23F 109.5 . . ? H23D C23' H23F 109.5 . . ? H23E C23' H23F 109.5 . . ? C22 C24' H24D 109.5 . . ? C22 C24' H24E 109.5 . . ? H24D C24' H24E 109.5 . . ? C22 C24' H24F 109.5 . . ? H24D C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? C22 C25' H25D 109.5 . . ? C22 C25' H25E 109.4 . . ? H25D C25' H25E 109.5 . . ? C22 C25' H25F 109.5 . . ? H25D C25' H25F 109.5 . . ? H25E C25' H25F 109.5 . . ? Si1 C26' H26A 109.5 . . ? Si1 C26' H26B 109.5 . . ? H26A C26' H26B 109.5 . . ? Si1 C26' H26C 109.5 . . ? H26A C26' H26C 109.5 . . ? H26B C26' H26C 109.5 . . ? Si1 C27' H27D 109.5 . . ? Si1 C27' H27E 109.5 . . ? H27D C27' H27E 109.5 . . ? Si1 C27' H27F 109.5 . . ? H27D C27' H27F 109.5 . . ? H27E C27' H27F 109.5 . . ? Si1 C28' H28D 109.5 . . ? Si1 C28' H28E 109.5 . . ? H28D C28' H28E 109.5 . . ? Si1 C28' H28F 109.5 . . ? H28D C28' H28F 109.5 . . ? H28E C28' H28F 109.5 . . ? Si2 C29' H29A 109.5 . . ? Si2 C29' H29B 109.5 . . ? H29A C29' H29B 109.5 . . ? Si2 C29' H29C 109.5 . . ? H29A C29' H29C 109.5 . . ? H29B C29' H29C 109.5 . . ? Si2 C30' H30D 109.5 . . ? Si2 C30' H30E 109.5 . . ? H30D C30' H30E 109.5 . . ? Si2 C30' H30F 109.5 . . ? H30D C30' H30F 109.5 . . ? H30E C30' H30F 109.5 . . ? Si2 C31' H31A 109.5 . . ? Si2 C31' H31B 109.5 . . ? H31A C31' H31B 109.5 . . ? Si2 C31' H31C 109.5 . . ? H31A C31' H31C 109.5 . . ? H31B C31' H31C 109.5 . . ? _refine_diff_density_max 0.761 _refine_diff_density_min -0.858 _refine_diff_density_rms 0.097 _shelxl_version_number 2013-4 _shelx_res_file ; TITL mo_dm11445_0m in P-1 CELL 0.71073 11.4423 13.3701 14.0720 61.692 87.288 70.508 ZERR 1.00 0.0065 0.0079 0.0078 0.011 0.012 0.011 LATT 1 SFAC C H N O Mg Si Br UNIT 62 88 6 2 2 4 2 OMIT -3 52 L.S. 8 ACTA wpdb -1 BOND $H FMAP 2 PLAN 8 SIZE 0.120 0.150 0.250 sadi 0.01 si1 c26 si1 c27 si1 c28 si1 c26' si1 c27' si1 c28' simu 0.01 c22 > last isor 0.01 c22 > last dfix 1.54 0.02 c22 c23 c22 c24 c22 c25 c22 c23' c22 c24' c22 c25' TEMP 23.000 WGHT 0.156400 FVAR 0.20562 BR1 7 0.659587 0.624010 0.579387 11.00000 0.09300 0.05374 = 0.08660 -0.00354 0.05066 0.00101 MG1 5 1.014765 0.494334 0.610689 11.00000 0.04301 0.03677 = 0.03591 -0.01884 0.00229 -0.00791 N1 3 1.024685 0.668742 0.285612 11.00000 0.03882 0.04500 = 0.03559 -0.02033 0.00544 -0.01035 N2 3 1.091639 0.977246 0.127571 11.00000 0.10195 0.05221 = 0.06702 -0.01976 -0.00494 -0.02662 N3 3 1.095299 0.544942 0.695479 11.00000 0.05793 0.05671 = 0.05334 -0.03558 0.00418 -0.01992 O1 4 0.897300 0.592736 0.471810 11.00000 0.03937 0.03579 = 0.03955 -0.01744 -0.00120 -0.00014 SI1 6 1.023998 0.677431 0.699020 11.00000 0.07822 0.06669 = 0.07867 -0.05007 0.00330 -0.02207 SI2 6 1.239934 0.448682 0.770393 11.00000 0.06309 0.07710 = 0.06075 -0.03812 -0.00555 -0.01920 C1 1 0.815119 0.704986 0.418872 11.00000 0.04011 0.04114 = 0.03564 -0.01823 -0.00055 -0.00594 C2 1 0.700025 0.744090 0.451749 11.00000 0.04952 0.04358 = 0.04580 -0.01716 0.00989 -0.00591 C3 1 0.614232 0.859398 0.400472 11.00000 0.04681 0.05209 = 0.04907 -0.01948 0.01374 -0.00138 AFIX 43 H3 2 0.537622 0.877354 0.425855 11.00000 -1.20000 AFIX 0 C4 1 0.641750 0.950643 0.309563 11.00000 0.04441 0.04708 = 0.05056 -0.01920 0.00487 -0.00260 C5 1 0.757053 0.915714 0.274866 11.00000 0.05034 0.03949 = 0.05012 -0.01516 0.00865 -0.01079 AFIX 43 H5 2 0.778007 0.974550 0.214948 11.00000 -1.20000 AFIX 0 C6 1 0.842465 0.797038 0.325491 11.00000 0.03889 0.03747 = 0.04531 -0.01953 0.00450 -0.00942 C7 1 0.953893 0.772125 0.271878 11.00000 0.04239 0.04371 = 0.04310 -0.01741 0.00527 -0.01145 AFIX 43 H7 2 0.974575 0.838672 0.223074 11.00000 -1.20000 AFIX 0 C8 1 1.123911 0.663950 0.218816 11.00000 0.04192 0.04013 = 0.03614 -0.01398 0.00348 -0.00481 C9 1 1.127149 0.601146 0.162696 11.00000 0.05713 0.05883 = 0.05606 -0.03416 0.00885 -0.01434 AFIX 43 H9 2 1.064134 0.570731 0.165442 11.00000 -1.20000 AFIX 0 C10 1 1.223981 0.583790 0.102738 11.00000 0.07874 0.07587 = 0.06157 -0.04464 0.02530 -0.02246 AFIX 43 H10 2 1.226763 0.540429 0.066445 11.00000 -1.20000 AFIX 0 C11 1 1.315205 0.630264 0.096924 11.00000 0.07227 0.09891 = 0.07323 -0.04856 0.03406 -0.02623 AFIX 43 H11 2 1.379571 0.619771 0.055788 11.00000 -1.20000 AFIX 0 C12 1 1.311747 0.691959 0.151437 11.00000 0.05223 0.08555 = 0.07003 -0.03942 0.01625 -0.02209 AFIX 43 H12 2 1.376566 0.720335 0.148325 11.00000 -1.20000 AFIX 0 C13 1 1.216644 0.715004 0.211612 11.00000 0.03825 0.05782 = 0.04217 -0.01911 0.00694 -0.01297 C14 1 1.222403 0.778152 0.273984 11.00000 0.04398 0.06396 = 0.05348 -0.02730 0.01020 -0.02395 C15 1 1.291027 0.711428 0.375634 11.00000 0.06642 0.07669 = 0.05937 -0.02562 -0.00413 -0.02227 AFIX 43 H15 2 1.331402 0.628272 0.403280 11.00000 -1.20000 AFIX 0 C16 1 1.302899 0.762409 0.439022 11.00000 0.09040 0.12501 = 0.06143 -0.03560 -0.00302 -0.04696 AFIX 43 H16 2 1.351925 0.714941 0.506737 11.00000 -1.20000 AFIX 0 C17 1 1.240183 0.885176 0.399067 11.00000 0.12122 0.10728 = 0.08489 -0.05552 0.02161 -0.07049 AFIX 43 H17 2 1.243682 0.921119 0.441007 11.00000 -1.20000 AFIX 0 C18 1 1.173957 0.952574 0.299116 11.00000 0.11464 0.07195 = 0.07262 -0.03677 0.01388 -0.05159 AFIX 43 H18 2 1.133034 1.035369 0.273170 11.00000 -1.20000 AFIX 0 C19 1 1.163759 0.904688 0.233004 11.00000 0.07388 0.06381 = 0.06214 -0.02826 0.01225 -0.03993 C20 1 1.166104 1.002339 0.041451 11.00000 0.15871 0.08829 = 0.06810 -0.01712 0.01112 -0.04555 AFIX 137 H20A 2 1.214623 1.046255 0.046759 11.00000 -1.50000 H20B 2 1.112893 1.050343 -0.027142 11.00000 -1.50000 H20C 2 1.221161 0.927392 0.046488 11.00000 -1.50000 AFIX 0 C21 1 0.991356 1.092775 0.110613 11.00000 0.15242 0.05444 = 0.12597 -0.03022 -0.03047 -0.02131 AFIX 137 H21A 2 0.956776 1.079470 0.177269 11.00000 -1.50000 H21B 2 0.926542 1.117661 0.054724 11.00000 -1.50000 H21C 2 1.026612 1.155083 0.089002 11.00000 -1.50000 AFIX 0 C22 1 0.546999 1.080526 0.251461 11.00000 0.06315 0.05312 = 0.07747 -0.01252 0.01481 -0.00057 PART 1 C23 1 0.532009 1.132439 0.333336 10.50000 0.12514 0.05110 = 0.10687 -0.03868 0.01257 0.02051 AFIX 33 H23A 2 0.605906 1.089671 0.385701 10.50000 -1.50000 H23B 2 0.460801 1.121862 0.370313 10.50000 -1.50000 H23C 2 0.520215 1.217311 0.293717 10.50000 -1.50000 AFIX 0 C24 1 0.423900 1.079132 0.212268 10.50000 0.05167 0.10214 = 0.11113 0.00950 -0.00848 -0.00207 AFIX 33 H24A 2 0.440018 1.046516 0.163168 10.50000 -1.50000 H24B 2 0.364124 1.160465 0.175446 10.50000 -1.50000 H24C 2 0.391107 1.029548 0.273848 10.50000 -1.50000 AFIX 0 C25 1 0.588568 1.168584 0.149722 10.50000 0.08683 0.05560 = 0.07216 -0.01034 0.01771 0.00733 AFIX 33 H25A 2 0.596988 1.142641 0.095961 10.50000 -1.50000 H25B 2 0.667520 1.169076 0.169333 10.50000 -1.50000 H25C 2 0.527104 1.248914 0.120465 10.50000 -1.50000 AFIX 0 C26 1 0.939965 0.799010 0.558609 10.50000 0.12432 0.07705 = 0.14957 -0.07008 -0.02904 -0.00529 AFIX 33 H26D 2 0.924499 0.877578 0.551397 10.50000 -1.50000 H26E 2 0.861847 0.791149 0.548133 10.50000 -1.50000 H26F 2 0.990803 0.790151 0.504871 10.50000 -1.50000 AFIX 0 C27 1 0.920250 0.680783 0.805668 10.50000 0.09006 0.11015 = 0.17373 -0.08863 0.06201 -0.04015 AFIX 33 H27A 2 0.928891 0.736589 0.827030 10.50000 -1.50000 H27B 2 0.943986 0.601021 0.867918 10.50000 -1.50000 H27C 2 0.834811 0.706453 0.776603 10.50000 -1.50000 AFIX 0 C28 1 1.139332 0.749305 0.704129 10.50000 0.12726 0.04595 = 0.08956 -0.03269 0.00883 -0.03391 AFIX 33 H28A 2 1.106460 0.798271 0.738445 10.50000 -1.50000 H28B 2 1.152647 0.799312 0.631416 10.50000 -1.50000 H28C 2 1.217317 0.686743 0.745114 10.50000 -1.50000 AFIX 0 C29 1 1.370570 0.463913 0.685509 10.50000 0.07595 0.13581 = 0.11458 -0.01757 0.00223 -0.00804 AFIX 33 H29D 2 1.442449 0.451149 0.728154 10.50000 -1.50000 H29E 2 1.344786 0.543850 0.623366 10.50000 -1.50000 H29F 2 1.391452 0.404548 0.661488 10.50000 -1.50000 AFIX 0 C30 1 1.273243 0.281466 0.834186 10.50000 0.10545 0.06586 = 0.11924 -0.04733 -0.03789 -0.00595 AFIX 33 H30A 2 1.342492 0.238310 0.891272 10.50000 -1.50000 H30B 2 1.293550 0.256387 0.779999 10.50000 -1.50000 H30C 2 1.200757 0.264014 0.863978 10.50000 -1.50000 AFIX 0 C31 1 1.278492 0.458137 0.894452 10.50000 0.14982 0.11661 = 0.08846 -0.05469 -0.04134 -0.00615 AFIX 33 H31D 2 1.367638 0.430231 0.911528 10.50000 -1.50000 H31E 2 1.244938 0.408151 0.955094 10.50000 -1.50000 H31F 2 1.242470 0.540828 0.879698 10.50000 -1.50000 AFIX 0 PART 2 C23' 1 0.443258 1.107129 0.314935 10.50000 0.09520 0.05411 = 0.11792 -0.02266 0.03284 0.01890 AFIX 33 H23D 2 0.376631 1.084926 0.301633 10.50000 -1.50000 H23E 2 0.412483 1.192261 0.292523 10.50000 -1.50000 H23F 2 0.474305 1.061214 0.391248 10.50000 -1.50000 AFIX 0 C24' 1 0.487648 1.086198 0.149968 10.50000 0.11490 0.11248 = 0.11253 -0.01335 -0.03043 0.01505 AFIX 33 H24D 2 0.544354 1.025363 0.135170 10.50000 -1.50000 H24E 2 0.471895 1.165029 0.087867 10.50000 -1.50000 H24F 2 0.410377 1.071674 0.164764 10.50000 -1.50000 AFIX 0 C25' 1 0.606818 1.173704 0.209723 10.50000 0.11115 0.04881 = 0.15096 -0.01892 0.01034 0.00591 AFIX 33 H25D 2 0.640012 1.180006 0.143972 10.50000 -1.50000 H25E 2 0.673362 1.150644 0.263364 10.50000 -1.50000 H25F 2 0.545776 1.250735 0.194832 10.50000 -1.50000 AFIX 0 C26' 1 0.858221 0.756785 0.626523 10.50000 0.10049 0.08802 = 0.12159 -0.07549 -0.02383 0.01019 AFIX 33 H26A 2 0.819406 0.829170 0.632078 10.50000 -1.50000 H26B 2 0.811673 0.703574 0.659526 10.50000 -1.50000 H26C 2 0.859450 0.777884 0.551174 10.50000 -1.50000 AFIX 0 C27' 1 0.983335 0.639155 0.841663 10.50000 0.09577 0.09617 = 0.12474 -0.09269 0.03495 -0.03128 AFIX 33 H27D 2 0.989491 0.698906 0.858709 10.50000 -1.50000 H27E 2 1.040459 0.560458 0.893081 10.50000 -1.50000 H27F 2 0.899493 0.638745 0.845332 10.50000 -1.50000 AFIX 0 C28' 1 1.097037 0.796019 0.659087 10.50000 0.16716 0.06933 = 0.13108 -0.04607 0.05861 -0.03545 AFIX 33 H28D 2 1.079368 0.829472 0.707537 10.50000 -1.50000 H28E 2 1.063183 0.859469 0.585824 10.50000 -1.50000 H28F 2 1.185916 0.759768 0.663475 10.50000 -1.50000 AFIX 0 C29' 1 1.348188 0.400750 0.683419 10.50000 0.07318 0.13660 = 0.10470 -0.07304 -0.00097 -0.01746 AFIX 33 H29A 2 1.433088 0.379559 0.710912 10.50000 -1.50000 H29B 2 1.329122 0.466455 0.609873 10.50000 -1.50000 H29C 2 1.337797 0.331689 0.684928 10.50000 -1.50000 AFIX 0 C30' 1 1.226226 0.304915 0.883179 10.50000 0.08757 0.10785 = 0.09424 -0.02064 -0.02381 -0.01984 AFIX 33 H30D 2 1.287830 0.272108 0.944265 10.50000 -1.50000 H30E 2 1.239641 0.246968 0.858179 10.50000 -1.50000 H30F 2 1.144195 0.322133 0.904782 10.50000 -1.50000 AFIX 0 C31' 1 1.324086 0.512962 0.824508 10.50000 0.11122 0.14313 = 0.14400 -0.09816 -0.01760 -0.03659 AFIX 33 H31A 2 1.392757 0.448255 0.878411 10.50000 -1.50000 H31B 2 1.267540 0.555436 0.856916 10.50000 -1.50000 H31C 2 1.355217 0.568237 0.766012 10.50000 -1.50000 PART 0 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM mo_dm11445_0m in P-1 REM R1 = 0.0638 for 4143 Fo > 4sig(Fo) and 0.1154 for all 6899 data REM 435 parameters refined using 249 restraints END WGHT 0.1548 0.0000 REM Highest difference peak 0.761, deepest hole -0.858, 1-sigma level 0.097 Q1 1 0.6607 0.6067 0.5290 11.00000 0.05 0.76 Q2 1 0.7221 0.6251 0.5973 11.00000 0.05 0.71 Q3 1 0.6102 1.1278 0.3476 11.00000 0.05 0.44 Q4 1 1.2608 0.7608 0.4479 11.00000 0.05 0.43 Q5 1 0.5008 1.1092 0.3426 11.00000 0.05 0.42 Q6 1 0.6182 1.1565 0.2806 11.00000 0.05 0.38 Q7 1 1.1750 0.4463 0.9254 11.00000 0.05 0.37 Q8 1 0.6261 0.6252 0.6002 11.00000 0.05 0.34 ; _shelx_res_checksum 42130 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