# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Philip Mountford' _publ_contact_author_email PHILIP.MOUNTFORD@CHEMISTRY.OXFORD.AC.UK _publ_section_title ; Sodium, magnesium and zinc complexes of mono(phenolate) heteroscorpionate ligands ; loop_ _publ_author_name 'Philip Mountford' 'Mariana Luna Barros' 'Michael G. Cushion' 'A. Daniel Schofield' 'Andrew D. Schwarz' # Attachment 'Revised_B813116C.CIF' data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 696837' # Local code ads43 _chemical_name_systematic ; Na2{(Me2pz)2C(C6H2(tBu)2O}2(THF)2 ; _publ_section_exptl_refinement ; No special details. The molecules lie across crystallographic inversion centers ; _chemical_melting_point ? _cell_length_a 10.9739(2) _cell_length_b 11.2192(3) _cell_length_c 11.9206(3) _cell_angle_alpha 77.4985(11) _cell_angle_beta 79.4223(11) _cell_angle_gamma 88.4467(12) _cell_volume 1408.38(6) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240 0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 1 _chemical_formula_sum 'C58 H86 N8 Na2 O4' _chemical_formula_moiety 'C58 H86 N8 Na2 O4' _chemical_compound_source ? _chemical_formula_weight 1005.36 _cell_measurement_reflns_used 5651 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_max 0.10 _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_meas ? _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 0.088 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.95 _exptl_absorpt_correction_T_max 1.00 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 10896 _reflns_number_total 6314 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_theta_min 5.137 _diffrn_reflns_theta_max 27.452 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.256 _diffrn_measured_fraction_theta_full 0.988 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -13 _reflns_limit_h_max 14 _reflns_limit_k_min -13 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _oxford_diffrn_Wilson_B_factor 2.35 _oxford_diffrn_Wilson_scale 1.65 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.22 _refine_diff_density_max 0.33 _refine_ls_number_reflns 4150 _refine_ls_number_restraints 0 _refine_ls_number_parameters 325 _refine_ls_wR_factor_ref 0.0430 _refine_ls_goodness_of_fit_ref 1.1255 _refine_ls_R_factor_all 0.0731 _refine_ls_wR_factor_all 0.0581 _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 4150 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_gt 0.0430 _refine_ls_shift/su_max 0.000208 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.900 0.210 0.753 0.673E-01 0.217 ; 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Na1 Na 0.04873(6) 0.36603(6) 0.54225(6) 0.0260 1.0000 Uani . . . . . . O1 O 0.06888(11) 0.51123(11) 0.36782(10) 0.0245 1.0000 Uani . . . . . . O2 O 0.20467(13) 0.24935(12) 0.61268(11) 0.0351 1.0000 Uani . . . . . . N1 N -0.03028(13) 0.20563(13) 0.46082(11) 0.0229 1.0000 Uani . . . . . . N2 N -0.09776(12) 0.25051(12) 0.37506(11) 0.0211 1.0000 Uani . . . . . . N3 N -0.07527(13) 0.21565(13) 0.14025(12) 0.0261 1.0000 Uani . . . . . . N4 N -0.08513(12) 0.32686(12) 0.17075(11) 0.0217 1.0000 Uani . . . . . . C1 C -0.10667(16) 0.12736(15) 0.54147(14) 0.0243 1.0000 Uani . . . . . . C2 C -0.22296(17) 0.12394(16) 0.50931(15) 0.0268 1.0000 Uani . . . . . . C3 C -0.21538(15) 0.20456(15) 0.40374(14) 0.0235 1.0000 Uani . . . . . . C4 C -0.06368(18) 0.05796(17) 0.64908(16) 0.0325 1.0000 Uani . . . . . . C5 C -0.31381(16) 0.24151(18) 0.33226(16) 0.0302 1.0000 Uani . . . . . . C6 C -0.12187(16) 0.23309(17) 0.04220(15) 0.0276 1.0000 Uani . . . . . . C7 C -0.16006(16) 0.35395(18) 0.00990(15) 0.0307 1.0000 Uani . . . . . . C8 C -0.13603(15) 0.41226(16) 0.09395(14) 0.0252 1.0000 Uani . . . . . . C9 C -0.12846(19) 0.1289(2) -0.01673(18) 0.0403 1.0000 Uani . . . . . . C10 C -0.15940(19) 0.54012(17) 0.10753(18) 0.0352 1.0000 Uani . . . . . . C11 C -0.04231(15) 0.34640(15) 0.27410(13) 0.0204 1.0000 Uani . . . . . . C12 C 0.09717(14) 0.35610(14) 0.25870(13) 0.0200 1.0000 Uani . . . . . . C13 C 0.14485(15) 0.44813(14) 0.30465(13) 0.0203 1.0000 Uani . . . . . . C14 C 0.27685(15) 0.46460(15) 0.28145(13) 0.0221 1.0000 Uani . . . . . . C15 C 0.34963(15) 0.38721(15) 0.22008(13) 0.0225 1.0000 Uani . . . . . . C16 C 0.30216(15) 0.29400(15) 0.17840(13) 0.0215 1.0000 Uani . . . . . . C17 C 0.17366(15) 0.28067(15) 0.19898(13) 0.0212 1.0000 Uani . . . . . . C18 C 0.33658(16) 0.56611(16) 0.32326(15) 0.0261 1.0000 Uani . . . . . . C19 C 0.30219(19) 0.54999(18) 0.45694(16) 0.0330 1.0000 Uani . . . . . . C20 C 0.29239(18) 0.69044(16) 0.26427(16) 0.0310 1.0000 Uani . . . . . . C21 C 0.47835(17) 0.56630(19) 0.29256(19) 0.0373 1.0000 Uani . . . . . . C22 C 0.38674(15) 0.20523(16) 0.11961(14) 0.0249 1.0000 Uani . . . . . . C23 C 0.4019(2) 0.0910(2) 0.21199(19) 0.0456 1.0000 Uani . . . . . . C24 C 0.3324(2) 0.1675(2) 0.0232(2) 0.0470 1.0000 Uani . . . . . . C25 C 0.51572(19) 0.2604(2) 0.06550(19) 0.0431 1.0000 Uani . . . . . . C26 C 0.2839(2) 0.18900(19) 0.53177(17) 0.0417 1.0000 Uani . . . . . . C27 C 0.37295(19) 0.1157(2) 0.6003(2) 0.0439 1.0000 Uani . . . . . . C28 C 0.2942(2) 0.0821(2) 0.72191(19) 0.0513 1.0000 Uani . . . . . . C29 C 0.2236(2) 0.1977(2) 0.72908(17) 0.0388 1.0000 Uani . . . . . . H21 H -0.2967 0.0732 0.5545 0.0330 1.0000 Uiso R . . . . . H51 H -0.3921 0.1950 0.3714 0.0383 1.0000 Uiso R . . . . . H52 H -0.3290 0.3310 0.3245 0.0383 1.0000 Uiso R . . . . . H53 H -0.2863 0.2236 0.2529 0.0383 1.0000 Uiso R . . . . . H71 H -0.1975 0.3903 -0.0601 0.0383 1.0000 Uiso R . . . . . H101 H -0.1971 0.5867 0.0412 0.0440 1.0000 Uiso R . . . . . H102 H -0.2173 0.5395 0.1829 0.0440 1.0000 Uiso R . . . . . H103 H -0.0791 0.5799 0.1081 0.0440 1.0000 Uiso R . . . . . H111 H -0.0764 0.4262 0.2892 0.0262 1.0000 Uiso R . . . . . H151 H 0.4417 0.3991 0.2048 0.0288 1.0000 Uiso R . . . . . H171 H 0.1359 0.2155 0.1703 0.0268 1.0000 Uiso R . . . . . H191 H 0.3419 0.6168 0.4818 0.0453 1.0000 Uiso R . . . . . H192 H 0.3322 0.4692 0.4954 0.0453 1.0000 Uiso R . . . . . H193 H 0.2101 0.5534 0.4804 0.0453 1.0000 Uiso R . . . . . H201 H 0.3309 0.7567 0.2909 0.0396 1.0000 Uiso R . . . . . H202 H 0.2001 0.6940 0.2856 0.0396 1.0000 Uiso R . . . . . H203 H 0.3172 0.7018 0.1776 0.0396 1.0000 Uiso R . . . . . H211 H 0.5130 0.6334 0.3210 0.0500 1.0000 Uiso R . . . . . H212 H 0.5098 0.4860 0.3306 0.0500 1.0000 Uiso R . . . . . H213 H 0.5048 0.5795 0.2059 0.0500 1.0000 Uiso R . . . . . H231 H 0.4568 0.0323 0.1748 0.0538 1.0000 Uiso R . . . . . H232 H 0.4397 0.1136 0.2748 0.0538 1.0000 Uiso R . . . . . H233 H 0.3187 0.0520 0.2467 0.0538 1.0000 Uiso R . . . . . H241 H 0.3897 0.1098 -0.0132 0.0683 1.0000 Uiso R . . . . . H242 H 0.3214 0.2416 -0.0378 0.0683 1.0000 Uiso R . . . . . H243 H 0.2502 0.1263 0.0575 0.0683 1.0000 Uiso R . . . . . H251 H 0.5679 0.2000 0.0282 0.0531 1.0000 Uiso R . . . . . H252 H 0.5557 0.2817 0.1276 0.0531 1.0000 Uiso R . . . . . H253 H 0.5076 0.3359 0.0050 0.0531 1.0000 Uiso R . . . . . H261 H 0.3290 0.2505 0.4643 0.0532 1.0000 Uiso R . . . . . H262 H 0.2335 0.1336 0.5023 0.0532 1.0000 Uiso R . . . . . H271 H 0.4464 0.1666 0.6001 0.0576 1.0000 Uiso R . . . . . H272 H 0.4016 0.0418 0.5692 0.0576 1.0000 Uiso R . . . . . H281 H 0.3464 0.0608 0.7837 0.0660 1.0000 Uiso R . . . . . H282 H 0.2367 0.0123 0.7283 0.0660 1.0000 Uiso R . . . . . H291 H 0.2732 0.2553 0.7568 0.0509 1.0000 Uiso R . . . . . H292 H 0.1422 0.1799 0.7834 0.0509 1.0000 Uiso R . . . . . H91 H -0.0794 0.1484 -0.0980 0.0532 1.0000 Uiso R . . . . . H92 H -0.0961 0.0528 0.0285 0.0532 1.0000 Uiso R . . . . . H93 H -0.2171 0.1148 -0.0204 0.0532 1.0000 Uiso R . . . . . H41 H -0.1163 0.0797 0.7194 0.0406 1.0000 Uiso R . . . . . H42 H 0.0247 0.0804 0.6457 0.0406 1.0000 Uiso R . . . . . H43 H -0.0709 -0.0317 0.6536 0.0406 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0313(4) 0.0246(3) 0.0243(3) -0.0079(3) -0.0084(3) 0.0065(3) O1 0.0254(6) 0.0266(6) 0.0230(6) -0.0098(5) -0.0037(5) 0.0039(5) O2 0.0420(8) 0.0342(7) 0.0306(7) -0.0088(6) -0.0107(6) 0.0150(6) N1 0.0261(7) 0.0246(7) 0.0188(6) -0.0040(6) -0.0073(5) 0.0021(6) N2 0.0222(7) 0.0238(7) 0.0178(6) -0.0034(5) -0.0058(5) 0.0009(5) N3 0.0261(7) 0.0293(8) 0.0262(7) -0.0110(6) -0.0080(6) 0.0036(6) N4 0.0224(7) 0.0238(7) 0.0200(6) -0.0049(5) -0.0072(5) 0.0026(5) C1 0.0296(9) 0.0220(8) 0.0211(8) -0.0050(6) -0.0040(7) 0.0006(7) C2 0.0297(9) 0.0248(8) 0.0255(8) -0.0059(7) -0.0031(7) -0.0031(7) C3 0.0225(8) 0.0253(8) 0.0240(8) -0.0085(7) -0.0038(6) -0.0015(6) C4 0.0379(10) 0.0315(10) 0.0269(9) -0.0010(8) -0.0087(8) -0.0001(8) C5 0.0231(9) 0.0383(10) 0.0298(9) -0.0063(8) -0.0074(7) -0.0023(7) C6 0.0220(8) 0.0397(10) 0.0237(8) -0.0120(7) -0.0048(7) 0.0005(7) C7 0.0269(9) 0.0425(11) 0.0230(8) -0.0031(8) -0.0102(7) 0.0000(8) C8 0.0205(8) 0.0305(9) 0.0220(8) 0.0012(7) -0.0057(6) 0.0013(7) C9 0.0394(11) 0.0534(13) 0.0380(11) -0.0254(10) -0.0144(9) 0.0061(9) C10 0.0373(10) 0.0282(9) 0.0385(10) 0.0009(8) -0.0129(8) 0.0064(8) C11 0.0215(8) 0.0211(8) 0.0192(7) -0.0042(6) -0.0049(6) 0.0012(6) C12 0.0206(8) 0.0219(8) 0.0171(7) -0.0028(6) -0.0042(6) 0.0018(6) C13 0.0228(8) 0.0216(8) 0.0159(7) -0.0022(6) -0.0044(6) 0.0017(6) C14 0.0250(8) 0.0236(8) 0.0189(7) -0.0046(6) -0.0068(6) -0.0002(6) C15 0.0202(8) 0.0278(8) 0.0197(7) -0.0045(7) -0.0047(6) 0.0002(6) C16 0.0227(8) 0.0254(8) 0.0169(7) -0.0050(6) -0.0052(6) 0.0041(6) C17 0.0232(8) 0.0227(8) 0.0184(7) -0.0044(6) -0.0057(6) 0.0013(6) C18 0.0263(9) 0.0265(9) 0.0284(9) -0.0086(7) -0.0087(7) -0.0004(7) C19 0.0421(11) 0.0327(10) 0.0301(9) -0.0113(8) -0.0159(8) -0.0011(8) C20 0.0377(10) 0.0253(9) 0.0310(9) -0.0072(7) -0.0075(8) -0.0020(8) C21 0.0285(10) 0.0402(11) 0.0494(12) -0.0189(9) -0.0117(9) -0.0046(8) C22 0.0214(8) 0.0306(9) 0.0239(8) -0.0082(7) -0.0047(6) 0.0047(7) C23 0.0492(13) 0.0389(11) 0.0414(11) -0.0021(9) -0.0006(10) 0.0204(10) C24 0.0436(12) 0.0631(14) 0.0521(13) -0.0424(12) -0.0220(10) 0.0236(11) C25 0.0331(11) 0.0512(13) 0.0431(11) -0.0197(10) 0.0092(9) 0.0005(9) C26 0.0538(13) 0.0378(11) 0.0314(10) -0.0090(9) -0.0025(9) 0.0151(10) C27 0.0329(11) 0.0473(12) 0.0571(13) -0.0222(11) -0.0109(10) 0.0095(9) C28 0.0635(15) 0.0522(14) 0.0423(12) -0.0099(10) -0.0237(11) 0.0245(12) C29 0.0421(11) 0.0462(12) 0.0308(10) -0.0104(9) -0.0129(8) 0.0103(9) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.7480(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Na1 . Na1 2_566 3.1788(13) yes Na1 . O1 2_566 2.1785(13) yes Na1 . O1 . 2.3261(13) yes Na1 . O2 . 2.2973(14) yes Na1 . N1 . 2.4662(15) yes Na1 . C13 . 2.7946(16) yes O1 . C13 . 1.3159(19) yes O2 . C26 . 1.445(2) yes O2 . C29 . 1.434(2) yes N1 . N2 . 1.3718(18) yes N1 . C1 . 1.333(2) yes N2 . C3 . 1.359(2) yes N2 . C11 . 1.477(2) yes N3 . N4 . 1.3694(19) yes N3 . C6 . 1.335(2) yes N4 . C8 . 1.359(2) yes N4 . C11 . 1.4566(19) yes C1 . C2 . 1.402(2) yes C1 . C4 . 1.498(2) yes C2 . C3 . 1.372(2) yes C2 . H21 . 1.000 no C3 . C5 . 1.492(2) yes C4 . H41 . 1.000 no C4 . H42 . 1.000 no C4 . H43 . 1.000 no C5 . H51 . 1.000 no C5 . H52 . 1.000 no C5 . H53 . 1.000 no C6 . C7 . 1.402(3) yes C6 . C9 . 1.498(3) yes C7 . C8 . 1.375(2) yes C7 . H71 . 1.000 no C8 . C10 . 1.488(3) yes C9 . H91 . 1.000 no C9 . H92 . 1.000 no C9 . H93 . 1.000 no C10 . H101 . 1.000 no C10 . H102 . 1.000 no C10 . H103 . 1.000 no C11 . C12 . 1.512(2) yes C11 . H111 . 1.000 no C12 . C13 . 1.421(2) yes C12 . C17 . 1.389(2) yes C13 . C14 . 1.433(2) yes C14 . C15 . 1.396(2) yes C14 . C18 . 1.543(2) yes C15 . C16 . 1.400(2) yes C15 . H151 . 1.000 no C16 . C17 . 1.393(2) yes C16 . C22 . 1.536(2) yes C17 . H171 . 1.000 no C18 . C19 . 1.540(2) yes C18 . C20 . 1.529(2) yes C18 . C21 . 1.531(3) yes C19 . H191 . 1.000 no C19 . H192 . 1.000 no C19 . H193 . 1.000 no C20 . H201 . 1.000 no C20 . H202 . 1.000 no C20 . H203 . 1.000 no C21 . H211 . 1.000 no C21 . H212 . 1.000 no C21 . H213 . 1.000 no C22 . C23 . 1.526(3) yes C22 . C24 . 1.527(2) yes C22 . C25 . 1.530(3) yes C23 . H231 . 1.000 no C23 . H232 . 1.000 no C23 . H233 . 1.000 no C24 . H241 . 1.000 no C24 . H242 . 1.000 no C24 . H243 . 1.000 no C25 . H251 . 1.000 no C25 . H252 . 1.000 no C25 . H253 . 1.000 no C26 . C27 . 1.502(3) yes C26 . H261 . 1.000 no C26 . H262 . 1.000 no C27 . C28 . 1.521(3) yes C27 . H271 . 1.000 no C27 . H272 . 1.000 no C28 . C29 . 1.503(3) yes C28 . H281 . 1.000 no C28 . H282 . 1.000 no C29 . H291 . 1.000 no C29 . H292 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Na1 2_566 Na1 . O1 2_566 47.03(3) yes Na1 2_566 Na1 . O1 . 43.26(3) yes O1 2_566 Na1 . O1 . 90.29(5) yes Na1 2_566 Na1 . O2 . 146.41(5) yes O1 2_566 Na1 . O2 . 125.65(5) yes O1 . Na1 . O2 . 126.33(5) yes Na1 2_566 Na1 . N1 . 115.79(4) yes O1 2_566 Na1 . N1 . 124.16(5) yes O1 . Na1 . N1 . 93.94(5) yes O2 . Na1 . N1 . 94.92(5) yes Na1 2_566 Na1 . C13 . 71.15(4) yes O1 2_566 Na1 . C13 . 118.17(5) yes O1 . Na1 . C13 . 27.91(4) yes O2 . Na1 . C13 . 103.79(5) yes N1 . Na1 . C13 . 79.32(5) yes Na1 . O1 . Na1 2_566 89.71(5) yes Na1 . O1 . C13 . 96.26(9) yes Na1 2_566 O1 . C13 . 173.54(11) yes Na1 . O2 . C26 . 116.54(11) yes Na1 . O2 . C29 . 132.25(11) yes C26 . O2 . C29 . 109.17(14) yes Na1 . N1 . N2 . 113.33(10) yes Na1 . N1 . C1 . 112.20(10) yes N2 . N1 . C1 . 104.97(13) yes N1 . N2 . C3 . 111.61(13) yes N1 . N2 . C11 . 119.19(12) yes C3 . N2 . C11 . 128.89(13) yes N4 . N3 . C6 . 104.41(14) yes N3 . N4 . C8 . 112.43(13) yes N3 . N4 . C11 . 121.52(13) yes C8 . N4 . C11 . 126.04(14) yes N1 . C1 . C2 . 110.84(14) yes N1 . C1 . C4 . 120.31(15) yes C2 . C1 . C4 . 128.84(16) yes C1 . C2 . C3 . 106.14(15) yes C1 . C2 . H21 . 126.9 no C3 . C2 . H21 . 127.0 no C2 . C3 . N2 . 106.39(14) yes C2 . C3 . C5 . 129.03(16) yes N2 . C3 . C5 . 124.55(15) yes C1 . C4 . H41 . 109.1 no C1 . C4 . H42 . 109.2 no H41 . C4 . H42 . 109.5 no C1 . C4 . H43 . 109.6 no H41 . C4 . H43 . 109.7 no H42 . C4 . H43 . 109.7 no C3 . C5 . H51 . 109.6 no C3 . C5 . H52 . 109.3 no H51 . C5 . H52 . 109.5 no C3 . C5 . H53 . 109.5 no H51 . C5 . H53 . 109.5 no H52 . C5 . H53 . 109.5 no N3 . C6 . C7 . 111.16(15) yes N3 . C6 . C9 . 119.77(17) yes C7 . C6 . C9 . 129.07(16) yes C6 . C7 . C8 . 106.17(15) yes C6 . C7 . H71 . 126.8 no C8 . C7 . H71 . 127.0 no C7 . C8 . N4 . 105.83(15) yes C7 . C8 . C10 . 130.64(16) yes N4 . C8 . C10 . 123.52(15) yes C6 . C9 . H91 . 110.5 no C6 . C9 . H92 . 110.5 no H91 . C9 . H92 . 109.5 no C6 . C9 . H93 . 108.6 no H91 . C9 . H93 . 108.9 no H92 . C9 . H93 . 108.9 no C8 . C10 . H101 . 109.9 no C8 . C10 . H102 . 109.3 no H101 . C10 . H102 . 109.5 no C8 . C10 . H103 . 109.2 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no N2 . C11 . N4 . 108.42(12) yes N2 . C11 . C12 . 113.38(12) yes N4 . C11 . C12 . 113.50(13) yes N2 . C11 . H111 . 107.1 no N4 . C11 . H111 . 107.1 no C12 . C11 . H111 . 107.0 no C11 . C12 . C13 . 116.70(14) yes C11 . C12 . C17 . 120.92(14) yes C13 . C12 . C17 . 122.35(15) yes C12 . C13 . O1 . 119.99(14) yes C12 . C13 . Na1 . 100.09(10) yes O1 . C13 . Na1 . 55.83(8) yes C12 . C13 . C14 . 116.85(14) yes O1 . C13 . C14 . 123.14(14) yes Na1 . C13 . C14 . 112.73(10) yes C13 . C14 . C15 . 118.54(14) yes C13 . C14 . C18 . 120.46(14) yes C15 . C14 . C18 . 121.00(15) yes C14 . C15 . C16 . 124.27(15) yes C14 . C15 . H151 . 117.9 no C16 . C15 . H151 . 117.8 no C15 . C16 . C17 . 116.72(14) yes C15 . C16 . C22 . 122.08(14) yes C17 . C16 . C22 . 121.09(15) yes C16 . C17 . C12 . 121.20(15) yes C16 . C17 . H171 . 119.3 no C12 . C17 . H171 . 119.5 no C14 . C18 . C19 . 111.12(14) yes C14 . C18 . C20 . 109.26(13) yes C19 . C18 . C20 . 109.49(14) yes C14 . C18 . C21 . 112.28(14) yes C19 . C18 . C21 . 106.82(15) yes C20 . C18 . C21 . 107.76(15) yes C18 . C19 . H191 . 109.6 no C18 . C19 . H192 . 109.4 no H191 . C19 . H192 . 109.5 no C18 . C19 . H193 . 109.4 no H191 . C19 . H193 . 109.5 no H192 . C19 . H193 . 109.5 no C18 . C20 . H201 . 109.7 no C18 . C20 . H202 . 109.4 no H201 . C20 . H202 . 109.5 no C18 . C20 . H203 . 109.3 no H201 . C20 . H203 . 109.5 no H202 . C20 . H203 . 109.5 no C18 . C21 . H211 . 109.5 no C18 . C21 . H212 . 109.4 no H211 . C21 . H212 . 109.5 no C18 . C21 . H213 . 109.4 no H211 . C21 . H213 . 109.5 no H212 . C21 . H213 . 109.5 no C16 . C22 . C23 . 108.55(14) yes C16 . C22 . C24 . 111.85(14) yes C23 . C22 . C24 . 108.53(18) yes C16 . C22 . C25 . 111.99(15) yes C23 . C22 . C25 . 108.02(16) yes C24 . C22 . C25 . 107.79(16) yes C22 . C23 . H231 . 109.4 no C22 . C23 . H232 . 109.7 no H231 . C23 . H232 . 109.5 no C22 . C23 . H233 . 109.3 no H231 . C23 . H233 . 109.5 no H232 . C23 . H233 . 109.5 no C22 . C24 . H241 . 109.7 no C22 . C24 . H242 . 109.4 no H241 . C24 . H242 . 109.5 no C22 . C24 . H243 . 109.3 no H241 . C24 . H243 . 109.5 no H242 . C24 . H243 . 109.5 no C22 . C25 . H251 . 109.6 no C22 . C25 . H252 . 109.7 no H251 . C25 . H252 . 109.5 no C22 . C25 . H253 . 109.1 no H251 . C25 . H253 . 109.5 no H252 . C25 . H253 . 109.5 no O2 . C26 . C27 . 105.80(16) yes O2 . C26 . H261 . 110.4 no C27 . C26 . H261 . 111.0 no O2 . C26 . H262 . 110.2 no C27 . C26 . H262 . 110.0 no H261 . C26 . H262 . 109.5 no C26 . C27 . C28 . 101.72(17) yes C26 . C27 . H271 . 110.9 no C28 . C27 . H271 . 110.9 no C26 . C27 . H272 . 111.8 no C28 . C27 . H272 . 111.9 no H271 . C27 . H272 . 109.5 no C27 . C28 . C29 . 101.66(18) yes C27 . C28 . H281 . 111.7 no C29 . C28 . H281 . 111.8 no C27 . C28 . H282 . 110.9 no C29 . C28 . H282 . 111.1 no H281 . C28 . H282 . 109.5 no C28 . C29 . O2 . 105.89(15) yes C28 . C29 . H291 . 110.1 no O2 . C29 . H291 . 110.2 no C28 . C29 . H292 . 110.8 no O2 . C29 . H292 . 110.3 no H291 . C29 . H292 . 109.5 no _chemical_name_common Na2((Me2pz)2C(C6H2(tBu)2O)2(THF)2 #===end data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 696838' # Local code ads28 _chemical_name_systematic ; Mg{(Me2pz)2C(C6H2(tBu)2O}Bu ; _publ_section_exptl_refinement ; H atoms were placed geometrically against orientations determined from a Fourier map. H atoms were refined in a riding model ; _chemical_melting_point ? _cell_length_a 11.2537(2) _cell_length_b 21.1315(5) _cell_length_c 23.8492(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5671.5(2) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,z x+1/2,-y+1/2,-z x,-y+1/2,z+1/2 -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 x+1/2,y,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Mg 0.0486 0.0363 5.4204 2.8275 2.1735 79.2611 1.2269 0.3808 2.3073 7.1937 0.8584 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 _chemical_formula_sum 'C29 H44 Mg1 N4 O1' _chemical_formula_moiety 'C29 H44 Mg1 N4 O1' _chemical_compound_source ? _chemical_formula_weight 489.00 _cell_measurement_reflns_used 5972 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 26.022 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_min 0.2 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_max 0.4 _exptl_crystal_density_diffrn 1.145 _exptl_crystal_density_meas ? _exptl_crystal_F_000 2128 _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.95 _exptl_absorpt_correction_T_max 0.95 _diffrn_measurement_device_type Unknown _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method /w _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 10777 _reflns_number_total 5521 _diffrn_reflns_av_R_equivalents 0.053 _diffrn_reflns_theta_min 5.156 _diffrn_reflns_theta_max 26.016 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.496 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _reflns_limit_h_min 0 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 26 _reflns_limit_l_min 0 _reflns_limit_l_max 29 _oxford_diffrn_Wilson_B_factor 2.42 _oxford_diffrn_Wilson_scale 14.88 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.26 _refine_diff_density_max 0.50 _refine_ls_number_reflns 3055 _refine_ls_number_restraints 0 _refine_ls_number_parameters 316 _refine_ls_wR_factor_ref 0.0594 _refine_ls_goodness_of_fit_ref 1.0938 _refine_ls_R_factor_all 0.1078 _refine_ls_wR_factor_all 0.0919 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 3055 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_gt 0.0594 _refine_ls_shift/su_max 0.000246 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.31 1.04 0.912 ; 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Mg1 Mg 0.77689(8) 0.65380(4) 0.43622(3) 0.0298 1.0000 Uani . . . . . . N1 N 0.61502(18) 0.60672(10) 0.41775(8) 0.0290 1.0000 Uani . . . . . . N2 N 0.61447(17) 0.54244(10) 0.42489(8) 0.0274 1.0000 Uani . . . . . . N3 N 0.80485(17) 0.58308(9) 0.49922(8) 0.0267 1.0000 Uani . . . . . . N4 N 0.78764(17) 0.52195(10) 0.48195(8) 0.0271 1.0000 Uani . . . . . . O1 O 0.87237(16) 0.60896(8) 0.38352(7) 0.0328 1.0000 Uani . . . . . . C1 C 0.5020(2) 0.62291(14) 0.40832(11) 0.0342 1.0000 Uani . . . . . . C2 C 0.4297(2) 0.56915(14) 0.40930(11) 0.0356 1.0000 Uani . . . . . . C3 C 0.5021(2) 0.51863(13) 0.41962(10) 0.0305 1.0000 Uani . . . . . . C4 C 0.4693(3) 0.69004(15) 0.39776(13) 0.0471 1.0000 Uani . . . . . . C5 C 0.4736(2) 0.45027(14) 0.42534(12) 0.0386 1.0000 Uani . . . . . . C6 C 0.8680(2) 0.57853(13) 0.54683(10) 0.0293 1.0000 Uani . . . . . . C7 C 0.8903(2) 0.51533(13) 0.55943(10) 0.0316 1.0000 Uani . . . . . . C8 C 0.8393(2) 0.47997(13) 0.51751(10) 0.0289 1.0000 Uani . . . . . . C9 C 0.9043(2) 0.63641(14) 0.57841(11) 0.0381 1.0000 Uani . . . . . . C10 C 0.8373(2) 0.41069(13) 0.50773(12) 0.0369 1.0000 Uani . . . . . . C11 C 0.7247(2) 0.50577(11) 0.42974(10) 0.0255 1.0000 Uani . . . . . . C12 C 0.8011(2) 0.50292(11) 0.37690(10) 0.0256 1.0000 Uani . . . . . . C13 C 0.8703(2) 0.55419(12) 0.35738(10) 0.0275 1.0000 Uani . . . . . . C14 C 0.9408(2) 0.54408(13) 0.30805(10) 0.0293 1.0000 Uani . . . . . . C15 C 0.9329(2) 0.48581(13) 0.28135(10) 0.0314 1.0000 Uani . . . . . . C16 C 0.8623(2) 0.43545(12) 0.29953(10) 0.0300 1.0000 Uani . . . . . . C17 C 0.7979(2) 0.44511(12) 0.34825(10) 0.0286 1.0000 Uani . . . . . . C18 C 1.0206(2) 0.59675(14) 0.28459(10) 0.0346 1.0000 Uani . . . . . . C19 C 1.1134(2) 0.61645(16) 0.32889(12) 0.0431 1.0000 Uani . . . . . . C20 C 0.9439(3) 0.65389(15) 0.26818(13) 0.0472 1.0000 Uani . . . . . . C21 C 1.0910(3) 0.57571(16) 0.23272(12) 0.0445 1.0000 Uani . . . . . . C22 C 0.8535(2) 0.37475(14) 0.26439(11) 0.0358 1.0000 Uani . . . . . . C23 C 0.7881(3) 0.32191(14) 0.29467(12) 0.0420 1.0000 Uani . . . . . . C24 C 0.9779(3) 0.35029(15) 0.24858(15) 0.0501 1.0000 Uani . . . . . . C25 C 0.7869(3) 0.39130(16) 0.21001(11) 0.0462 1.0000 Uani . . . . . . C26 C 0.7839(3) 0.75242(14) 0.45304(14) 0.0498 1.0000 Uani . . . . . . C27 C 0.8919(3) 0.78317(19) 0.4291(2) 0.0863 1.0000 Uani . . . . . . C28 C 1.0042(3) 0.75209(18) 0.44134(16) 0.0593 1.0000 Uani . . . . . . C29 C 1.1145(3) 0.7776(2) 0.4112(2) 0.0742 1.0000 Uani . . . . . . H21 H 0.3418 0.5680 0.4032 0.0460 1.0000 Uiso R . . . . . H41 H 0.5386 0.7181 0.4062 0.0595 1.0000 Uiso R . . . . . H42 H 0.4458 0.6953 0.3576 0.0595 1.0000 Uiso R . . . . . H43 H 0.4010 0.7020 0.4224 0.0595 1.0000 Uiso R . . . . . H51 H 0.3863 0.4439 0.4199 0.0492 1.0000 Uiso R . . . . . H52 H 0.4969 0.4353 0.4635 0.0492 1.0000 Uiso R . . . . . H53 H 0.5182 0.4257 0.3963 0.0492 1.0000 Uiso R . . . . . H71 H 0.9343 0.4989 0.5928 0.0409 1.0000 Uiso R . . . . . H91 H 0.9513 0.6243 0.6123 0.0498 1.0000 Uiso R . . . . . H92 H 0.9536 0.6641 0.5536 0.0498 1.0000 Uiso R . . . . . H93 H 0.8312 0.6598 0.5902 0.0498 1.0000 Uiso R . . . . . H101 H 0.8807 0.3886 0.5387 0.0471 1.0000 Uiso R . . . . . H102 H 0.8763 0.4008 0.4711 0.0471 1.0000 Uiso R . . . . . H103 H 0.7529 0.3959 0.5068 0.0471 1.0000 Uiso R . . . . . H111 H 0.6974 0.4612 0.4357 0.0348 1.0000 Uiso R . . . . . H151 H 0.9813 0.4794 0.2466 0.0399 1.0000 Uiso R . . . . . H171 H 0.7479 0.4098 0.3632 0.0377 1.0000 Uiso R . . . . . H191 H 1.1649 0.6507 0.3132 0.0574 1.0000 Uiso R . . . . . H192 H 1.0719 0.6323 0.3632 0.0574 1.0000 Uiso R . . . . . H193 H 1.1636 0.5791 0.3389 0.0574 1.0000 Uiso R . . . . . H201 H 0.9964 0.6880 0.2531 0.0606 1.0000 Uiso R . . . . . H202 H 0.9010 0.6698 0.3021 0.0606 1.0000 Uiso R . . . . . H203 H 0.8848 0.6413 0.2389 0.0606 1.0000 Uiso R . . . . . H211 H 1.1416 0.6115 0.2192 0.0604 1.0000 Uiso R . . . . . H212 H 1.1427 0.5390 0.2428 0.0604 1.0000 Uiso R . . . . . H213 H 1.0346 0.5629 0.2024 0.0604 1.0000 Uiso R . . . . . H231 H 0.7848 0.2837 0.2700 0.0535 1.0000 Uiso R . . . . . H232 H 0.8309 0.3112 0.3302 0.0535 1.0000 Uiso R . . . . . H233 H 0.7055 0.3360 0.3037 0.0535 1.0000 Uiso R . . . . . H241 H 0.9701 0.3107 0.2259 0.0692 1.0000 Uiso R . . . . . H242 H 1.0245 0.3412 0.2834 0.0692 1.0000 Uiso R . . . . . H243 H 1.0201 0.3832 0.2260 0.0692 1.0000 Uiso R . . . . . H251 H 0.7791 0.3526 0.1862 0.0597 1.0000 Uiso R . . . . . H252 H 0.8326 0.4244 0.1891 0.0597 1.0000 Uiso R . . . . . H253 H 0.7061 0.4079 0.2194 0.0597 1.0000 Uiso R . . . . . H261 H 0.7115 0.7766 0.4416 0.0656 1.0000 Uiso R . . . . . H262 H 0.7908 0.7527 0.4948 0.0656 1.0000 Uiso R . . . . . H271 H 0.8966 0.8279 0.4428 0.1202 1.0000 Uiso R . . . . . H272 H 0.8831 0.7829 0.3874 0.1202 1.0000 Uiso R . . . . . H281 H 1.0181 0.7573 0.4825 0.0793 1.0000 Uiso R . . . . . H282 H 0.9952 0.7061 0.4324 0.0793 1.0000 Uiso R . . . . . H291 H 1.1866 0.7535 0.4233 0.0948 1.0000 Uiso R . . . . . H292 H 1.1256 0.8235 0.4201 0.0948 1.0000 Uiso R . . . . . H293 H 1.1027 0.7723 0.3699 0.0948 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0294(4) 0.0270(4) 0.0330(4) 0.0000(4) 0.0007(4) 0.0001(4) N1 0.0249(11) 0.0304(12) 0.0316(11) -0.0035(9) -0.0020(9) 0.0047(9) N2 0.0198(10) 0.0323(12) 0.0299(10) -0.0029(9) 0.0009(8) 0.0006(9) N3 0.0242(10) 0.0269(11) 0.0290(10) -0.0023(9) 0.0011(8) -0.0030(9) N4 0.0219(10) 0.0308(11) 0.0286(10) -0.0014(9) 0.0026(8) 0.0005(9) O1 0.0328(10) 0.0320(10) 0.0337(9) -0.0009(8) 0.0057(8) -0.0029(8) C1 0.0301(14) 0.0426(16) 0.0298(13) -0.0063(11) -0.0011(11) 0.0084(13) C2 0.0259(13) 0.0506(18) 0.0303(13) -0.0086(12) 0.0014(11) 0.0070(13) C3 0.0212(12) 0.0445(16) 0.0257(12) -0.0052(11) 0.0034(9) -0.0020(12) C4 0.0422(16) 0.0497(19) 0.0495(17) -0.0066(14) -0.0069(13) 0.0170(15) C5 0.0292(13) 0.0437(16) 0.0428(15) -0.0066(13) 0.0059(12) -0.0083(12) C6 0.0204(11) 0.0398(15) 0.0278(12) -0.0017(11) 0.0043(10) -0.0023(11) C7 0.0238(12) 0.0418(16) 0.0293(12) 0.0046(11) 0.0001(10) 0.0034(11) C8 0.0228(12) 0.0351(14) 0.0289(12) 0.0069(11) 0.0046(10) 0.0040(11) C9 0.0339(14) 0.0453(17) 0.0350(14) -0.0039(12) -0.0022(11) -0.0034(13) C10 0.0354(14) 0.0358(15) 0.0395(14) 0.0051(12) 0.0017(12) 0.0043(12) C11 0.0196(11) 0.0264(12) 0.0305(12) -0.0003(10) -0.0006(9) 0.0000(10) C12 0.0193(11) 0.0302(13) 0.0273(12) -0.0001(10) -0.0018(10) 0.0015(10) C13 0.0200(11) 0.0311(13) 0.0315(13) 0.0019(11) -0.0042(10) 0.0040(11) C14 0.0202(12) 0.0398(15) 0.0279(12) 0.0055(11) -0.0017(9) 0.0005(11) C15 0.0215(12) 0.0455(16) 0.0273(12) -0.0019(12) 0.0026(10) 0.0023(12) C16 0.0212(12) 0.0383(15) 0.0306(12) -0.0036(11) -0.0044(10) 0.0045(11) C17 0.0204(11) 0.0317(13) 0.0339(13) 0.0001(11) -0.0029(10) 0.0019(11) C18 0.0299(13) 0.0457(17) 0.0282(13) 0.0043(12) 0.0032(11) -0.0019(12) C19 0.0321(15) 0.0585(19) 0.0387(15) 0.0009(14) 0.0029(12) -0.0126(14) C20 0.0427(16) 0.0496(18) 0.0494(17) 0.0170(14) 0.0049(14) -0.0005(14) C21 0.0369(15) 0.062(2) 0.0346(15) 0.0035(14) 0.0075(12) -0.0100(14) C22 0.0241(13) 0.0428(16) 0.0406(15) -0.0162(12) 0.0003(11) -0.0012(12) C23 0.0389(15) 0.0382(15) 0.0489(17) -0.0154(13) 0.0016(13) 0.0019(13) C24 0.0306(15) 0.0547(19) 0.065(2) -0.0251(17) 0.0025(13) 0.0025(14) C25 0.0369(16) 0.065(2) 0.0369(15) -0.0132(14) -0.0014(12) -0.0072(15) C26 0.0501(17) 0.0305(15) 0.069(2) 0.0001(14) 0.0048(16) -0.0010(14) C27 0.059(2) 0.045(2) 0.154(4) 0.020(2) 0.002(3) -0.0087(18) C28 0.0527(19) 0.056(2) 0.069(2) 0.0053(18) -0.0067(17) -0.0117(16) C29 0.055(2) 0.071(3) 0.097(3) 0.023(2) -0.004(2) -0.0076(19) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2565(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mg1 . N1 . 2.122(2) yes Mg1 . N3 . 2.142(2) yes Mg1 . O1 . 1.9058(19) yes Mg1 . C26 . 2.124(3) yes N1 . N2 . 1.369(3) yes N1 . C1 . 1.336(3) yes N2 . C3 . 1.367(3) yes N2 . C11 . 1.467(3) yes N3 . N4 . 1.370(3) yes N3 . C6 . 1.343(3) yes N4 . C8 . 1.358(3) yes N4 . C11 . 1.473(3) yes O1 . C13 . 1.315(3) yes C1 . C2 . 1.398(4) yes C1 . C4 . 1.487(4) yes C2 . C3 . 1.366(4) yes C2 . H21 . 1.000 no C3 . C5 . 1.486(4) yes C4 . H41 . 1.000 no C4 . H42 . 1.000 no C4 . H43 . 1.000 no C5 . H51 . 1.000 no C5 . H52 . 1.000 no C5 . H53 . 1.000 no C6 . C7 . 1.392(4) yes C6 . C9 . 1.493(4) yes C7 . C8 . 1.374(4) yes C7 . H71 . 1.000 no C8 . C10 . 1.483(4) yes C9 . H91 . 1.000 no C9 . H92 . 1.000 no C9 . H93 . 1.000 no C10 . H101 . 1.000 no C10 . H102 . 1.000 no C10 . H103 . 1.000 no C11 . C12 . 1.527(3) yes C11 . H111 . 1.000 no C12 . C13 . 1.413(4) yes C12 . C17 . 1.400(3) yes C13 . C14 . 1.435(3) yes C14 . C15 . 1.389(4) yes C14 . C18 . 1.535(4) yes C15 . C16 . 1.398(4) yes C15 . H151 . 1.000 no C16 . C17 . 1.384(3) yes C16 . C22 . 1.535(4) yes C17 . H171 . 1.000 no C18 . C19 . 1.543(4) yes C18 . C20 . 1.535(4) yes C18 . C21 . 1.535(4) yes C19 . H191 . 1.000 no C19 . H192 . 1.000 no C19 . H193 . 1.000 no C20 . H201 . 1.000 no C20 . H202 . 1.000 no C20 . H203 . 1.000 no C21 . H211 . 1.000 no C21 . H212 . 1.000 no C21 . H213 . 1.000 no C22 . C23 . 1.520(4) yes C22 . C24 . 1.539(4) yes C22 . C25 . 1.538(4) yes C23 . H231 . 1.000 no C23 . H232 . 1.000 no C23 . H233 . 1.000 no C24 . H241 . 1.000 no C24 . H242 . 1.000 no C24 . H243 . 1.000 no C25 . H251 . 1.000 no C25 . H252 . 1.000 no C25 . H253 . 1.000 no C26 . C27 . 1.491(5) yes C26 . H261 . 1.000 no C26 . H262 . 1.000 no C27 . C28 . 1.453(5) yes C27 . H271 . 1.000 no C27 . H272 . 1.000 no C28 . C29 . 1.533(5) yes C28 . H281 . 1.000 no C28 . H282 . 1.000 no C29 . H291 . 1.000 no C29 . H292 . 1.000 no C29 . H293 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Mg1 . N3 . 86.82(8) yes N1 . Mg1 . O1 . 96.55(8) yes N3 . Mg1 . O1 . 91.88(8) yes N1 . Mg1 . C26 . 122.08(11) yes N3 . Mg1 . C26 . 123.14(11) yes O1 . Mg1 . C26 . 126.27(11) yes Mg1 . N1 . N2 . 116.31(14) yes Mg1 . N1 . C1 . 137.06(19) yes N2 . N1 . C1 . 105.7(2) yes N1 . N2 . C3 . 111.0(2) yes N1 . N2 . C11 . 122.01(19) yes C3 . N2 . C11 . 126.5(2) yes Mg1 . N3 . N4 . 115.23(14) yes Mg1 . N3 . C6 . 136.10(17) yes N4 . N3 . C6 . 105.16(19) yes N3 . N4 . C8 . 111.58(19) yes N3 . N4 . C11 . 122.77(19) yes C8 . N4 . C11 . 125.6(2) yes Mg1 . O1 . C13 . 137.75(16) yes N1 . C1 . C2 . 110.1(2) yes N1 . C1 . C4 . 120.6(3) yes C2 . C1 . C4 . 129.3(2) yes C1 . C2 . C3 . 106.9(2) yes C1 . C2 . H21 . 126.4 no C3 . C2 . H21 . 126.7 no N2 . C3 . C2 . 106.3(2) yes N2 . C3 . C5 . 123.3(2) yes C2 . C3 . C5 . 130.4(2) yes C1 . C4 . H41 . 109.9 no C1 . C4 . H42 . 109.5 no H41 . C4 . H42 . 109.5 no C1 . C4 . H43 . 109.4 no H41 . C4 . H43 . 109.3 no H42 . C4 . H43 . 109.3 no C3 . C5 . H51 . 109.4 no C3 . C5 . H52 . 109.6 no H51 . C5 . H52 . 109.5 no C3 . C5 . H53 . 109.5 no H51 . C5 . H53 . 109.5 no H52 . C5 . H53 . 109.5 no N3 . C6 . C7 . 110.3(2) yes N3 . C6 . C9 . 120.8(2) yes C7 . C6 . C9 . 128.9(2) yes C6 . C7 . C8 . 106.8(2) yes C6 . C7 . H71 . 126.4 no C8 . C7 . H71 . 126.7 no C7 . C8 . N4 . 106.1(2) yes C7 . C8 . C10 . 131.1(2) yes N4 . C8 . C10 . 122.7(2) yes C6 . C9 . H91 . 110.1 no C6 . C9 . H92 . 109.5 no H91 . C9 . H92 . 109.5 no C6 . C9 . H93 . 108.8 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no C8 . C10 . H101 . 109.7 no C8 . C10 . H102 . 109.7 no H101 . C10 . H102 . 109.5 no C8 . C10 . H103 . 109.0 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no N4 . C11 . N2 . 110.52(18) yes N4 . C11 . C12 . 115.86(19) yes N2 . C11 . C12 . 115.60(19) yes N4 . C11 . H111 . 104.3 no N2 . C11 . H111 . 104.4 no C12 . C11 . H111 . 104.6 no C11 . C12 . C13 . 123.5(2) yes C11 . C12 . C17 . 115.0(2) yes C13 . C12 . C17 . 121.5(2) yes C12 . C13 . O1 . 121.9(2) yes C12 . C13 . C14 . 117.4(2) yes O1 . C13 . C14 . 120.6(2) yes C13 . C14 . C15 . 118.2(2) yes C13 . C14 . C18 . 120.9(2) yes C15 . C14 . C18 . 120.9(2) yes C14 . C15 . C16 . 124.7(2) yes C14 . C15 . H151 . 117.6 no C16 . C15 . H151 . 117.7 no C15 . C16 . C17 . 116.5(2) yes C15 . C16 . C22 . 120.2(2) yes C17 . C16 . C22 . 123.2(2) yes C12 . C17 . C16 . 121.6(2) yes C12 . C17 . H171 . 119.4 no C16 . C17 . H171 . 119.0 no C14 . C18 . C19 . 110.0(2) yes C14 . C18 . C20 . 109.5(2) yes C19 . C18 . C20 . 110.1(3) yes C14 . C18 . C21 . 112.7(2) yes C19 . C18 . C21 . 106.3(2) yes C20 . C18 . C21 . 108.2(2) yes C18 . C19 . H191 . 109.4 no C18 . C19 . H192 . 109.5 no H191 . C19 . H192 . 109.5 no C18 . C19 . H193 . 109.5 no H191 . C19 . H193 . 109.5 no H192 . C19 . H193 . 109.5 no C18 . C20 . H201 . 109.1 no C18 . C20 . H202 . 109.3 no H201 . C20 . H202 . 109.5 no C18 . C20 . H203 . 110.0 no H201 . C20 . H203 . 109.5 no H202 . C20 . H203 . 109.5 no C18 . C21 . H211 . 109.6 no C18 . C21 . H212 . 109.4 no H211 . C21 . H212 . 109.5 no C18 . C21 . H213 . 109.5 no H211 . C21 . H213 . 109.5 no H212 . C21 . H213 . 109.5 no C16 . C22 . C23 . 112.7(2) yes C16 . C22 . C24 . 110.9(2) yes C23 . C22 . C24 . 108.1(2) yes C16 . C22 . C25 . 107.6(2) yes C23 . C22 . C25 . 109.4(2) yes C24 . C22 . C25 . 108.2(2) yes C22 . C23 . H231 . 109.4 no C22 . C23 . H232 . 109.6 no H231 . C23 . H232 . 109.5 no C22 . C23 . H233 . 109.5 no H231 . C23 . H233 . 109.5 no H232 . C23 . H233 . 109.5 no C22 . C24 . H241 . 109.4 no C22 . C24 . H242 . 109.7 no H241 . C24 . H242 . 109.5 no C22 . C24 . H243 . 109.2 no H241 . C24 . H243 . 109.5 no H242 . C24 . H243 . 109.5 no C22 . C25 . H251 . 109.6 no C22 . C25 . H252 . 109.2 no H251 . C25 . H252 . 109.5 no C22 . C25 . H253 . 109.6 no H251 . C25 . H253 . 109.5 no H252 . C25 . H253 . 109.5 no Mg1 . C26 . C27 . 112.7(3) yes Mg1 . C26 . H261 . 114.8 no C27 . C26 . H261 . 109.7 no Mg1 . C26 . H262 . 101.4 no C27 . C26 . H262 . 108.4 no H261 . C26 . H262 . 109.5 no C26 . C27 . C28 . 115.8(3) yes C26 . C27 . H271 . 109.3 no C28 . C27 . H271 . 108.4 no C26 . C27 . H272 . 107.3 no C28 . C27 . H272 . 106.4 no H271 . C27 . H272 . 109.5 no C27 . C28 . C29 . 116.9(3) yes C27 . C28 . H281 . 106.4 no C29 . C28 . H281 . 107.1 no C27 . C28 . H282 . 108.0 no C29 . C28 . H282 . 108.9 no H281 . C28 . H282 . 109.5 no C28 . C29 . H291 . 110.1 no C28 . C29 . H292 . 110.0 no H291 . C29 . H292 . 109.5 no C28 . C29 . H293 . 108.2 no H291 . C29 . H293 . 109.5 no H292 . C29 . H293 . 109.5 no _chemical_name_common Mg((Me2pz)2C(C6H2(tBu)2O)Bu #===end data_compound_4.C4H10O _database_code_depnum_ccdc_archive 'CCDC 696839' # Local code ads54 _chemical_name_systematic ; Mg{(Me2pz)2C(C6H2(tBu)2O}2 . OEt2 ; _publ_section_exptl_refinement ; Similarity restraints were applied to the displacement parameter of the Et2O solvent molecule. The crystal was a thin plate and a relatively weak diffractor (mean I/s(I) ca 5.5) ; _chemical_melting_point ? _cell_length_a 15.7496(4) _cell_length_b 17.6620(5) _cell_length_c 20.2696(5) _cell_angle_alpha 90 _cell_angle_beta 92.8818(17) _cell_angle_gamma 90 _cell_volume 5631.3(3) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source Mg 0.0486 0.0363 5.4204 2.8275 2.1735 79.2611 1.2269 0.3808 2.3073 7.1937 0.8584 'International Tables Vol C 4.2.6.8 and 6.1.1.4' C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C54 H80 Mg1 N8 O3' _chemical_formula_moiety 'C50 H70 Mg1 N8 O2 , C4 H10 O' _chemical_compound_source ? _chemical_formula_weight 913.59 _cell_measurement_reflns_used 9336 _cell_measurement_theta_min 5 _cell_measurement_theta_max 25 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour white _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.078 _exptl_crystal_density_meas ? _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.98 _exptl_absorpt_correction_T_max 0.99 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 17019 _reflns_number_total 9832 _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_theta_min 5.166 _diffrn_reflns_theta_max 25.030 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.030 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min -18 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _oxford_diffrn_Wilson_B_factor 2.81 _oxford_diffrn_Wilson_scale 28.40 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.42 _refine_diff_density_max 0.93 _refine_ls_number_reflns 5266 _refine_ls_number_restraints 21 _refine_ls_number_parameters 595 _refine_ls_wR_factor_ref 0.0879 _refine_ls_goodness_of_fit_ref 1.1015 _refine_ls_R_factor_all 0.1472 _refine_ls_wR_factor_all 0.1249 _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 5266 _refine_ls_R_factor_gt 0.0826 _refine_ls_wR_factor_gt 0.0879 _refine_ls_shift/su_max 0.000396 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.34 0.676 0.973 -0.383E-01 0.150 ; 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Mg1 Mg 0.83722(9) 0.68468(8) 0.61102(7) 0.0261 1.0000 Uani . . . . . . O1 O 0.96223(17) 0.67463(18) 0.62225(14) 0.0279 1.0000 Uani . . . . . . O2 O 0.80590(19) 0.62226(17) 0.68624(14) 0.0298 1.0000 Uani . . . . . . O3 O 0.4982(3) 0.4542(3) 0.6548(3) 0.0821 1.0000 Uani . U . . . . N1 N 0.8452(2) 0.5987(2) 0.53261(17) 0.0286 1.0000 Uani . . . . . . N2 N 0.9082(2) 0.6061(2) 0.48913(17) 0.0266 1.0000 Uani . . . . . . N3 N 0.8484(2) 0.7683(2) 0.52396(18) 0.0316 1.0000 Uani . . . . . . N4 N 0.8862(2) 0.7385(2) 0.47011(17) 0.0293 1.0000 Uani . . . . . . N5 N 0.8156(2) 0.7846(2) 0.67164(18) 0.0284 1.0000 Uani . . . . . . N6 N 0.7433(2) 0.7908(2) 0.70634(17) 0.0277 1.0000 Uani . . . . . . N7 N 0.6936(2) 0.6978(2) 0.58394(18) 0.0312 1.0000 Uani . . . . . . N8 N 0.6437(2) 0.7283(2) 0.63090(17) 0.0290 1.0000 Uani . . . . . . C1 C 0.8136(3) 0.5300(3) 0.5220(2) 0.0337 1.0000 Uani . . . . . . C2 C 0.8571(3) 0.4918(3) 0.4729(2) 0.0359 1.0000 Uani . . . . . . C3 C 0.9173(3) 0.5418(3) 0.4529(2) 0.0306 1.0000 Uani . . . . . . C4 C 0.7399(3) 0.5018(3) 0.5591(3) 0.0409 1.0000 Uani . . . . . . C5 C 0.9836(3) 0.5344(3) 0.4030(2) 0.0381 1.0000 Uani . . . . . . C6 C 0.7997(3) 0.8250(3) 0.4989(2) 0.0351 1.0000 Uani . . . . . . C7 C 0.8062(3) 0.8306(3) 0.4306(2) 0.0394 1.0000 Uani . . . . . . C8 C 0.8614(3) 0.7748(3) 0.4133(2) 0.0336 1.0000 Uani . . . . . . C9 C 0.7477(3) 0.8746(3) 0.5402(3) 0.0442 1.0000 Uani . . . . . . C10 C 0.8922(3) 0.7526(3) 0.3470(2) 0.0413 1.0000 Uani . . . . . . C11 C 0.9500(3) 0.6788(3) 0.4772(2) 0.0264 1.0000 Uani . . . . . . C12 C 1.0282(3) 0.6968(3) 0.5210(2) 0.0264 1.0000 Uani . . . . . . C13 C 1.0307(3) 0.6903(2) 0.5906(2) 0.0262 1.0000 Uani . . . . . . C14 C 1.1124(3) 0.7012(3) 0.6245(2) 0.0276 1.0000 Uani . . . . . . C15 C 1.1794(3) 0.7249(3) 0.5876(2) 0.0310 1.0000 Uani . . . . . . C16 C 1.1757(3) 0.7352(3) 0.5196(2) 0.0354 1.0000 Uani . . . . . . C17 C 1.0988(3) 0.7187(3) 0.4871(2) 0.0321 1.0000 Uani . . . . . . C18 C 1.1268(3) 0.6827(3) 0.6985(2) 0.0300 1.0000 Uani . . . . . . C19 C 1.0699(3) 0.7312(3) 0.7413(2) 0.0374 1.0000 Uani . . . . . . C20 C 1.1074(3) 0.5994(3) 0.7093(2) 0.0406 1.0000 Uani . . . . . . C21 C 1.2187(3) 0.6973(4) 0.7231(2) 0.0462 1.0000 Uani . . . . . . C22 C 1.2551(3) 0.7622(4) 0.4849(2) 0.0506 1.0000 Uani . . . . . . C23 C 1.2817(4) 0.8400(4) 0.5106(3) 0.0612 1.0000 Uani . . . . . . C24 C 1.3277(4) 0.7081(5) 0.4978(3) 0.0713 1.0000 Uani . . . . . . C25 C 1.2382(4) 0.7663(6) 0.4094(3) 0.0828 1.0000 Uani . . . . . . C26 C 0.8594(3) 0.8469(3) 0.6852(2) 0.0349 1.0000 Uani . . . . . . C27 C 0.8169(3) 0.8930(3) 0.7289(2) 0.0371 1.0000 Uani . . . . . . C28 C 0.7426(3) 0.8567(3) 0.7413(2) 0.0367 1.0000 Uani . . . . . . C29 C 0.9415(3) 0.8638(3) 0.6529(3) 0.0415 1.0000 Uani . . . . . . C30 C 0.6719(4) 0.8777(3) 0.7838(3) 0.0549 1.0000 Uani . . . . . . C31 C 0.6427(3) 0.6953(3) 0.5287(2) 0.0371 1.0000 Uani . . . . . . C32 C 0.5626(3) 0.7220(3) 0.5409(3) 0.0462 1.0000 Uani . . . . . . C33 C 0.5637(3) 0.7441(3) 0.6060(2) 0.0399 1.0000 Uani . . . . . . C34 C 0.6706(3) 0.6682(4) 0.4639(2) 0.0456 1.0000 Uani . . . . . . C35 C 0.4964(4) 0.7773(4) 0.6457(3) 0.0550 1.0000 Uani . . . . . . C36 C 0.6728(3) 0.7368(3) 0.6996(2) 0.0289 1.0000 Uani . . . . . . C37 C 0.6816(3) 0.6632(2) 0.7381(2) 0.0266 1.0000 Uani . . . . . . C38 C 0.7490(3) 0.6118(3) 0.7306(2) 0.0269 1.0000 Uani . . . . . . C39 C 0.7515(3) 0.5471(3) 0.7740(2) 0.0291 1.0000 Uani . . . . . . C40 C 0.6842(3) 0.5361(3) 0.8146(2) 0.0309 1.0000 Uani . . . . . . C41 C 0.6153(3) 0.5838(3) 0.8195(2) 0.0308 1.0000 Uani . . . . . . C42 C 0.6169(3) 0.6490(3) 0.7809(2) 0.0334 1.0000 Uani . . . . . . C43 C 0.8300(3) 0.4942(3) 0.7778(2) 0.0351 1.0000 Uani . . . . . . C44 C 0.8409(4) 0.4545(3) 0.7115(3) 0.0439 1.0000 Uani . . . . . . C45 C 0.8223(3) 0.4334(3) 0.8311(3) 0.0432 1.0000 Uani . . . . . . C46 C 0.9091(3) 0.5415(3) 0.7955(3) 0.0433 1.0000 Uani . . . . . . C47 C 0.5414(3) 0.5682(3) 0.8634(2) 0.0409 1.0000 Uani . U . . . . C48 C 0.5314(4) 0.6331(4) 0.9121(3) 0.0685 1.0000 Uani . U . . . . C49 C 0.4600(5) 0.5615(6) 0.8214(4) 0.0921 1.0000 Uani . U . . . . C50 C 0.5552(5) 0.4965(4) 0.9049(4) 0.0779 1.0000 Uani . U . . . . C51 C 0.4082(8) 0.5569(6) 0.6258(6) 0.1237 1.0000 Uani . U . . . . C52 C 0.4971(7) 0.5278(6) 0.6272(5) 0.1047 1.0000 Uani . U . . . . C53 C 0.5791(5) 0.4226(5) 0.6591(5) 0.0914 1.0000 Uani . U . . . . C54 C 0.5811(6) 0.3512(6) 0.6928(5) 0.1067 1.0000 Uani . U . . . . H21 H 0.8465 0.4391 0.4564 0.0451 1.0000 Uiso R . . . . . H41 H 0.7254 0.4489 0.5450 0.0588 1.0000 Uiso R . . . . . H42 H 0.7556 0.5025 0.6075 0.0588 1.0000 Uiso R . . . . . H43 H 0.6897 0.5354 0.5497 0.0588 1.0000 Uiso R . . . . . H51 H 0.9792 0.4832 0.3820 0.0490 1.0000 Uiso R . . . . . H52 H 1.0415 0.5408 0.4249 0.0490 1.0000 Uiso R . . . . . H53 H 0.9741 0.5743 0.3684 0.0490 1.0000 Uiso R . . . . . H71 H 0.7765 0.8677 0.4001 0.0495 1.0000 Uiso R . . . . . H91 H 0.7162 0.9125 0.5117 0.0560 1.0000 Uiso R . . . . . H92 H 0.7861 0.9015 0.5733 0.0560 1.0000 Uiso R . . . . . H93 H 0.7061 0.8430 0.5638 0.0560 1.0000 Uiso R . . . . . H101 H 0.8663 0.7869 0.3122 0.0562 1.0000 Uiso R . . . . . H102 H 0.9555 0.7569 0.3476 0.0562 1.0000 Uiso R . . . . . H103 H 0.8750 0.6992 0.3371 0.0562 1.0000 Uiso R . . . . . H111 H 0.9721 0.6733 0.4320 0.0344 1.0000 Uiso R . . . . . H151 H 1.2348 0.7352 0.6123 0.0409 1.0000 Uiso R . . . . . H171 H 1.0938 0.7222 0.4378 0.0423 1.0000 Uiso R . . . . . H191 H 1.0813 0.7177 0.7889 0.0531 1.0000 Uiso R . . . . . H192 H 1.0828 0.7860 0.7346 0.0531 1.0000 Uiso R . . . . . H193 H 1.0087 0.7213 0.7285 0.0531 1.0000 Uiso R . . . . . H201 H 1.1167 0.5869 0.7573 0.0538 1.0000 Uiso R . . . . . H202 H 1.1454 0.5672 0.6829 0.0538 1.0000 Uiso R . . . . . H203 H 1.0467 0.5895 0.6951 0.0538 1.0000 Uiso R . . . . . H211 H 1.2254 0.6849 0.7712 0.0618 1.0000 Uiso R . . . . . H212 H 1.2333 0.7517 0.7162 0.0618 1.0000 Uiso R . . . . . H213 H 1.2574 0.6645 0.6979 0.0618 1.0000 Uiso R . . . . . H231 H 1.3329 0.8576 0.4876 0.0769 1.0000 Uiso R . . . . . H232 H 1.2956 0.8367 0.5592 0.0769 1.0000 Uiso R . . . . . H233 H 1.2341 0.8767 0.5020 0.0769 1.0000 Uiso R . . . . . H241 H 1.3796 0.7253 0.4756 0.0874 1.0000 Uiso R . . . . . H242 H 1.3408 0.7044 0.5465 0.0874 1.0000 Uiso R . . . . . H243 H 1.3099 0.6573 0.4802 0.0874 1.0000 Uiso R . . . . . H251 H 1.2903 0.7846 0.3880 0.1027 1.0000 Uiso R . . . . . H252 H 1.1899 0.8015 0.3982 0.1027 1.0000 Uiso R . . . . . H253 H 1.2235 0.7143 0.3929 0.1027 1.0000 Uiso R . . . . . H271 H 0.8362 0.9430 0.7472 0.0467 1.0000 Uiso R . . . . . H291 H 0.9648 0.9134 0.6693 0.0534 1.0000 Uiso R . . . . . H292 H 0.9834 0.8226 0.6641 0.0534 1.0000 Uiso R . . . . . H293 H 0.9307 0.8662 0.6039 0.0534 1.0000 Uiso R . . . . . H301 H 0.6845 0.9281 0.8045 0.0742 1.0000 Uiso R . . . . . H302 H 0.6658 0.8388 0.8191 0.0742 1.0000 Uiso R . . . . . H303 H 0.6178 0.8808 0.7559 0.0742 1.0000 Uiso R . . . . . H321 H 0.5127 0.7245 0.5085 0.0575 1.0000 Uiso R . . . . . H341 H 0.7304 0.6492 0.4686 0.0592 1.0000 Uiso R . . . . . H342 H 0.6325 0.6267 0.4465 0.0592 1.0000 Uiso R . . . . . H343 H 0.6680 0.7113 0.4319 0.0592 1.0000 Uiso R . . . . . H351 H 0.4429 0.7839 0.6175 0.0692 1.0000 Uiso R . . . . . H352 H 0.5158 0.8277 0.6632 0.0692 1.0000 Uiso R . . . . . H353 H 0.4854 0.7428 0.6834 0.0692 1.0000 Uiso R . . . . . H361 H 0.6247 0.7635 0.7202 0.0385 1.0000 Uiso R . . . . . H401 H 0.6857 0.4897 0.8429 0.0413 1.0000 Uiso R . . . . . H421 H 0.5707 0.6874 0.7848 0.0425 1.0000 Uiso R . . . . . H441 H 0.8918 0.4207 0.7155 0.0593 1.0000 Uiso R . . . . . H442 H 0.8491 0.4932 0.6763 0.0593 1.0000 Uiso R . . . . . H443 H 0.7892 0.4235 0.6995 0.0593 1.0000 Uiso R . . . . . H451 H 0.8741 0.4006 0.8324 0.0558 1.0000 Uiso R . . . . . H452 H 0.8167 0.4576 0.8753 0.0558 1.0000 Uiso R . . . . . H453 H 0.7709 0.4020 0.8199 0.0558 1.0000 Uiso R . . . . . H461 H 0.9602 0.5079 0.7984 0.0569 1.0000 Uiso R . . . . . H462 H 0.9029 0.5675 0.8388 0.0569 1.0000 Uiso R . . . . . H463 H 0.9160 0.5803 0.7602 0.0569 1.0000 Uiso R . . . . . H481 H 0.4829 0.6223 0.9407 0.0936 1.0000 Uiso R . . . . . H482 H 0.5849 0.6392 0.9403 0.0936 1.0000 Uiso R . . . . . H483 H 0.5197 0.6808 0.8866 0.0936 1.0000 Uiso R . . . . . H491 H 0.4119 0.5515 0.8507 0.1216 1.0000 Uiso R . . . . . H492 H 0.4492 0.6098 0.7966 0.1216 1.0000 Uiso R . . . . . H493 H 0.4647 0.5188 0.7895 0.1216 1.0000 Uiso R . . . . . H501 H 0.5053 0.4892 0.9329 0.1021 1.0000 Uiso R . . . . . H502 H 0.6084 0.4996 0.9338 0.1021 1.0000 Uiso R . . . . . H503 H 0.5592 0.4527 0.8740 0.1021 1.0000 Uiso R . . . . . H511 H 0.4078 0.6089 0.6063 0.1466 1.0000 Uiso R . . . . . H512 H 0.3880 0.5594 0.6718 0.1466 1.0000 Uiso R . . . . . H513 H 0.3697 0.5232 0.5983 0.1466 1.0000 Uiso R . . . . . H521 H 0.5357 0.5613 0.6548 0.1173 1.0000 Uiso R . . . . . H522 H 0.5175 0.5251 0.5813 0.1173 1.0000 Uiso R . . . . . H531 H 0.6171 0.4591 0.6841 0.1099 1.0000 Uiso R . . . . . H532 H 0.5984 0.4160 0.6136 0.1099 1.0000 Uiso R . . . . . H541 H 0.6411 0.3325 0.6942 0.1240 1.0000 Uiso R . . . . . H542 H 0.5622 0.3570 0.7389 0.1240 1.0000 Uiso R . . . . . H543 H 0.5434 0.3139 0.6684 0.1240 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0245(7) 0.0284(8) 0.0259(7) -0.0004(6) 0.0045(5) -0.0006(6) O1 0.0237(15) 0.0342(17) 0.0263(15) 0.0013(14) 0.0050(12) -0.0035(13) O2 0.0294(16) 0.0317(17) 0.0291(16) 0.0022(13) 0.0091(13) -0.0001(14) O3 0.083(3) 0.077(3) 0.088(3) 0.016(3) 0.021(3) -0.023(3) N1 0.0269(19) 0.032(2) 0.0274(19) -0.0032(16) 0.0041(15) -0.0014(17) N2 0.0215(18) 0.033(2) 0.0259(19) -0.0045(16) 0.0046(15) -0.0032(16) N3 0.033(2) 0.033(2) 0.030(2) -0.0021(17) 0.0069(16) 0.0022(18) N4 0.032(2) 0.035(2) 0.0213(19) 0.0031(16) 0.0055(15) -0.0006(17) N5 0.0267(19) 0.031(2) 0.028(2) 0.0016(16) 0.0032(15) -0.0020(17) N6 0.032(2) 0.0232(19) 0.029(2) -0.0012(15) 0.0058(16) 0.0029(16) N7 0.0258(19) 0.039(2) 0.029(2) 0.0004(17) 0.0027(16) -0.0009(17) N8 0.0245(19) 0.036(2) 0.0266(19) 0.0033(17) 0.0041(15) 0.0011(17) C1 0.031(2) 0.039(3) 0.032(2) -0.003(2) 0.0034(19) -0.005(2) C2 0.040(3) 0.035(3) 0.033(3) -0.009(2) 0.002(2) -0.008(2) C3 0.031(2) 0.035(3) 0.025(2) -0.005(2) -0.0023(18) 0.002(2) C4 0.041(3) 0.041(3) 0.041(3) -0.006(2) 0.012(2) -0.013(2) C5 0.036(3) 0.049(3) 0.030(3) -0.013(2) 0.008(2) 0.001(2) C6 0.031(2) 0.038(3) 0.035(3) 0.005(2) 0.001(2) 0.005(2) C7 0.040(3) 0.046(3) 0.033(3) 0.014(2) 0.004(2) 0.002(2) C8 0.027(2) 0.046(3) 0.028(2) 0.009(2) 0.0038(18) 0.001(2) C9 0.049(3) 0.040(3) 0.044(3) 0.004(2) 0.008(2) 0.015(2) C10 0.045(3) 0.052(3) 0.027(2) 0.005(2) 0.003(2) 0.001(3) C11 0.022(2) 0.036(3) 0.022(2) 0.0028(19) 0.0041(16) -0.0010(19) C12 0.025(2) 0.026(2) 0.028(2) -0.0018(18) 0.0028(17) -0.0012(19) C13 0.023(2) 0.023(2) 0.033(2) -0.0030(19) 0.0023(18) 0.0007(19) C14 0.028(2) 0.027(2) 0.028(2) -0.0046(18) 0.0034(18) 0.0002(19) C15 0.026(2) 0.037(3) 0.030(2) -0.009(2) 0.0032(18) 0.001(2) C16 0.027(2) 0.048(3) 0.032(3) -0.006(2) 0.0053(19) -0.007(2) C17 0.027(2) 0.040(3) 0.029(2) -0.003(2) 0.0033(19) -0.005(2) C18 0.031(2) 0.034(3) 0.025(2) 0.000(2) 0.0023(18) -0.002(2) C19 0.046(3) 0.041(3) 0.025(2) -0.008(2) 0.003(2) 0.001(2) C20 0.049(3) 0.039(3) 0.034(3) 0.006(2) -0.003(2) 0.002(2) C21 0.041(3) 0.068(4) 0.029(3) -0.002(3) -0.003(2) -0.004(3) C22 0.037(3) 0.083(4) 0.033(3) -0.011(3) 0.011(2) -0.026(3) C23 0.053(4) 0.082(5) 0.049(3) -0.003(3) 0.012(3) -0.036(3) C24 0.033(3) 0.111(6) 0.071(4) -0.039(4) 0.014(3) -0.016(3) C25 0.056(4) 0.164(8) 0.030(3) -0.012(4) 0.016(3) -0.056(5) C26 0.033(3) 0.032(3) 0.039(3) 0.005(2) -0.004(2) -0.001(2) C27 0.042(3) 0.029(3) 0.040(3) -0.003(2) 0.002(2) -0.003(2) C28 0.046(3) 0.029(2) 0.036(3) -0.005(2) 0.007(2) 0.006(2) C29 0.029(3) 0.036(3) 0.060(3) 0.002(2) 0.004(2) -0.006(2) C30 0.066(4) 0.047(3) 0.053(3) -0.014(3) 0.021(3) 0.002(3) C31 0.033(3) 0.045(3) 0.032(3) -0.002(2) -0.001(2) -0.003(2) C32 0.031(3) 0.068(4) 0.039(3) 0.004(3) -0.005(2) 0.003(3) C33 0.027(2) 0.055(3) 0.038(3) 0.005(2) 0.003(2) 0.010(2) C34 0.040(3) 0.066(4) 0.030(3) -0.002(3) -0.003(2) 0.000(3) C35 0.039(3) 0.079(4) 0.046(3) -0.006(3) -0.001(2) 0.021(3) C36 0.023(2) 0.033(3) 0.031(2) -0.002(2) 0.0062(18) -0.001(2) C37 0.029(2) 0.025(2) 0.026(2) -0.0017(18) 0.0043(17) -0.0006(19) C38 0.032(2) 0.027(2) 0.022(2) 0.0006(18) 0.0022(18) -0.004(2) C39 0.032(2) 0.027(2) 0.029(2) 0.0032(19) 0.0048(18) -0.0009(19) C40 0.033(2) 0.029(2) 0.031(2) -0.001(2) 0.0074(19) -0.005(2) C41 0.032(2) 0.028(3) 0.033(2) -0.006(2) 0.0066(19) -0.005(2) C42 0.035(3) 0.035(3) 0.032(2) -0.004(2) 0.009(2) -0.001(2) C43 0.037(3) 0.033(3) 0.037(3) 0.008(2) 0.011(2) 0.005(2) C44 0.050(3) 0.034(3) 0.049(3) 0.002(2) 0.016(2) 0.010(2) C45 0.042(3) 0.038(3) 0.050(3) 0.012(2) 0.011(2) 0.009(2) C46 0.037(3) 0.042(3) 0.051(3) 0.010(3) 0.004(2) 0.004(2) C47 0.036(3) 0.048(3) 0.041(3) 0.000(2) 0.016(2) -0.003(2) C48 0.065(4) 0.080(5) 0.063(4) 0.002(4) 0.028(3) 0.006(4) C49 0.060(4) 0.136(7) 0.082(5) 0.009(5) 0.016(4) -0.035(5) C50 0.082(5) 0.071(5) 0.084(5) 0.021(4) 0.042(4) 0.000(4) C51 0.159(8) 0.097(6) 0.114(6) 0.028(6) -0.013(6) -0.018(6) C52 0.127(6) 0.085(5) 0.103(5) 0.016(5) 0.016(5) -0.024(5) C53 0.069(4) 0.098(5) 0.110(5) 0.004(4) 0.036(4) -0.009(4) C54 0.080(5) 0.118(7) 0.127(7) 0.032(6) 0.051(5) 0.016(5) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2254(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mg1 . O1 . 1.979(3) yes Mg1 . O2 . 1.964(3) yes Mg1 . N1 . 2.206(4) yes Mg1 . N3 . 2.315(4) yes Mg1 . N5 . 2.187(4) yes Mg1 . N7 . 2.312(4) yes O1 . C13 . 1.312(5) yes O2 . C38 . 1.314(5) yes O3 . C52 . 1.415(10) yes O3 . C53 . 1.390(10) yes N1 . N2 . 1.367(5) yes N1 . C1 . 1.324(6) yes N2 . C3 . 1.364(6) yes N2 . C11 . 1.468(6) yes N3 . N4 . 1.374(5) yes N3 . C6 . 1.346(6) yes N4 . C8 . 1.358(6) yes N4 . C11 . 1.459(6) yes N5 . N6 . 1.373(5) yes N5 . C26 . 1.320(6) yes N6 . C28 . 1.363(6) yes N6 . C36 . 1.465(6) yes N7 . N8 . 1.375(5) yes N7 . C31 . 1.345(6) yes N8 . C33 . 1.362(6) yes N8 . C36 . 1.453(6) yes C1 . C2 . 1.408(7) yes C1 . C4 . 1.501(6) yes C2 . C3 . 1.372(7) yes C2 . H21 . 1.000 no C3 . C5 . 1.495(6) yes C4 . H41 . 1.000 no C4 . H42 . 1.000 no C4 . H43 . 1.000 no C5 . H51 . 1.000 no C5 . H52 . 1.000 no C5 . H53 . 1.000 no C6 . C7 . 1.397(7) yes C6 . C9 . 1.486(7) yes C7 . C8 . 1.371(7) yes C7 . H71 . 1.000 no C8 . C10 . 1.503(7) yes C9 . H91 . 1.000 no C9 . H92 . 1.000 no C9 . H93 . 1.000 no C10 . H101 . 1.000 no C10 . H102 . 1.000 no C10 . H103 . 1.000 no C11 . C12 . 1.515(6) yes C11 . H111 . 1.000 no C12 . C13 . 1.414(6) yes C12 . C17 . 1.390(6) yes C13 . C14 . 1.441(6) yes C14 . C15 . 1.389(6) yes C14 . C18 . 1.540(6) yes C15 . C16 . 1.389(7) yes C15 . H151 . 1.000 no C16 . C17 . 1.379(6) yes C16 . C22 . 1.541(6) yes C17 . H171 . 1.000 no C18 . C19 . 1.539(6) yes C18 . C20 . 1.521(7) yes C18 . C21 . 1.529(7) yes C19 . H191 . 1.000 no C19 . H192 . 1.000 no C19 . H193 . 1.000 no C20 . H201 . 1.000 no C20 . H202 . 1.000 no C20 . H203 . 1.000 no C21 . H211 . 1.000 no C21 . H212 . 1.000 no C21 . H213 . 1.000 no C22 . C23 . 1.520(9) yes C22 . C24 . 1.504(10) yes C22 . C25 . 1.542(8) yes C23 . H231 . 1.000 no C23 . H232 . 1.000 no C23 . H233 . 1.000 no C24 . H241 . 1.000 no C24 . H242 . 1.000 no C24 . H243 . 1.000 no C25 . H251 . 1.000 no C25 . H252 . 1.000 no C25 . H253 . 1.000 no C26 . C27 . 1.398(7) yes C26 . C29 . 1.508(7) yes C27 . C28 . 1.369(7) yes C27 . H271 . 1.000 no C28 . C30 . 1.487(7) yes C29 . H291 . 1.000 no C29 . H292 . 1.000 no C29 . H293 . 1.000 no C30 . H301 . 1.000 no C30 . H302 . 1.000 no C30 . H303 . 1.000 no C31 . C32 . 1.380(7) yes C31 . C34 . 1.485(7) yes C32 . C33 . 1.375(7) yes C32 . H321 . 1.000 no C33 . C35 . 1.484(7) yes C34 . H341 . 1.000 no C34 . H342 . 1.000 no C34 . H343 . 1.000 no C35 . H351 . 1.000 no C35 . H352 . 1.000 no C35 . H353 . 1.000 no C36 . C37 . 1.518(6) yes C36 . H361 . 1.000 no C37 . C38 . 1.410(6) yes C37 . C42 . 1.393(6) yes C38 . C39 . 1.443(6) yes C39 . C40 . 1.389(6) yes C39 . C43 . 1.547(7) yes C40 . C41 . 1.382(7) yes C40 . H401 . 1.000 no C41 . C42 . 1.393(7) yes C41 . C47 . 1.525(6) yes C42 . H421 . 1.000 no C43 . C44 . 1.535(7) yes C43 . C45 . 1.533(7) yes C43 . C46 . 1.528(7) yes C44 . H441 . 1.000 no C44 . H442 . 1.000 no C44 . H443 . 1.000 no C45 . H451 . 1.000 no C45 . H452 . 1.000 no C45 . H453 . 1.000 no C46 . H461 . 1.000 no C46 . H462 . 1.000 no C46 . H463 . 1.000 no C47 . C48 . 1.526(9) yes C47 . C49 . 1.507(10) yes C47 . C50 . 1.531(9) yes C48 . H481 . 1.000 no C48 . H482 . 1.000 no C48 . H483 . 1.000 no C49 . H491 . 1.000 no C49 . H492 . 1.000 no C49 . H493 . 1.000 no C50 . H501 . 1.000 no C50 . H502 . 1.000 no C50 . H503 . 1.000 no C51 . C52 . 1.490(15) yes C51 . H511 . 1.000 no C51 . H512 . 1.000 no C51 . H513 . 1.000 no C52 . H521 . 1.000 no C52 . H522 . 1.000 no C53 . C54 . 1.434(12) yes C53 . H531 . 1.000 no C53 . H532 . 0.992 no C54 . H541 . 1.000 no C54 . H542 . 1.000 no C54 . H543 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . Mg1 . O2 . 98.49(14) yes O1 . Mg1 . N1 . 85.93(14) yes O2 . Mg1 . N1 . 101.44(14) yes O1 . Mg1 . N3 . 91.81(14) yes O2 . Mg1 . N3 . 168.96(15) yes N1 . Mg1 . N3 . 83.15(14) yes O1 . Mg1 . N5 . 100.94(14) yes O2 . Mg1 . N5 . 87.98(14) yes N1 . Mg1 . N5 . 167.49(15) yes N3 . Mg1 . N5 . 86.17(14) yes O1 . Mg1 . N7 . 172.84(14) yes O2 . Mg1 . N7 . 87.68(14) yes N1 . Mg1 . N7 . 89.30(14) yes N3 . Mg1 . N7 . 82.31(14) yes N5 . Mg1 . N7 . 82.81(14) yes Mg1 . O1 . C13 . 139.7(3) yes Mg1 . O2 . C38 . 144.7(3) yes C52 . O3 . C53 . 112.8(7) yes Mg1 . N1 . N2 . 117.9(3) yes Mg1 . N1 . C1 . 135.5(3) yes N2 . N1 . C1 . 105.2(3) yes N1 . N2 . C3 . 111.5(4) yes N1 . N2 . C11 . 122.5(3) yes C3 . N2 . C11 . 125.4(3) yes Mg1 . N3 . N4 . 114.5(3) yes Mg1 . N3 . C6 . 134.4(3) yes N4 . N3 . C6 . 104.3(4) yes N3 . N4 . C8 . 112.1(4) yes N3 . N4 . C11 . 121.5(3) yes C8 . N4 . C11 . 126.3(4) yes Mg1 . N5 . N6 . 120.6(3) yes Mg1 . N5 . C26 . 134.1(3) yes N6 . N5 . C26 . 105.4(4) yes N5 . N6 . C28 . 111.3(4) yes N5 . N6 . C36 . 123.1(3) yes C28 . N6 . C36 . 125.3(4) yes Mg1 . N7 . N8 . 117.5(3) yes Mg1 . N7 . C31 . 136.9(3) yes N8 . N7 . C31 . 104.5(4) yes N7 . N8 . C33 . 112.0(4) yes N7 . N8 . C36 . 122.7(3) yes C33 . N8 . C36 . 125.1(4) yes N1 . C1 . C2 . 111.2(4) yes N1 . C1 . C4 . 121.1(4) yes C2 . C1 . C4 . 127.7(4) yes C1 . C2 . C3 . 105.6(4) yes C1 . C2 . H21 . 127.0 no C3 . C2 . H21 . 127.4 no C2 . C3 . N2 . 106.5(4) yes C2 . C3 . C5 . 131.3(4) yes N2 . C3 . C5 . 122.2(4) yes C1 . C4 . H41 . 109.8 no C1 . C4 . H42 . 109.2 no H41 . C4 . H42 . 109.5 no C1 . C4 . H43 . 109.4 no H41 . C4 . H43 . 109.5 no H42 . C4 . H43 . 109.5 no C3 . C5 . H51 . 109.3 no C3 . C5 . H52 . 109.9 no H51 . C5 . H52 . 109.5 no C3 . C5 . H53 . 109.1 no H51 . C5 . H53 . 109.5 no H52 . C5 . H53 . 109.5 no N3 . C6 . C7 . 111.0(4) yes N3 . C6 . C9 . 123.0(4) yes C7 . C6 . C9 . 126.0(5) yes C6 . C7 . C8 . 106.4(4) yes C6 . C7 . H71 . 127.0 no C8 . C7 . H71 . 126.6 no C7 . C8 . N4 . 106.3(4) yes C7 . C8 . C10 . 130.7(4) yes N4 . C8 . C10 . 122.9(4) yes C6 . C9 . H91 . 109.9 no C6 . C9 . H92 . 109.0 no H91 . C9 . H92 . 109.5 no C6 . C9 . H93 . 109.5 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no C8 . C10 . H101 . 109.5 no C8 . C10 . H102 . 109.6 no H101 . C10 . H102 . 109.5 no C8 . C10 . H103 . 109.2 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no N2 . C11 . N4 . 109.6(3) yes N2 . C11 . C12 . 116.4(3) yes N4 . C11 . C12 . 116.2(4) yes N2 . C11 . H111 . 104.2 no N4 . C11 . H111 . 104.4 no C12 . C11 . H111 . 104.3 no C11 . C12 . C13 . 123.2(4) yes C11 . C12 . C17 . 114.6(4) yes C13 . C12 . C17 . 122.2(4) yes C12 . C13 . O1 . 121.6(4) yes C12 . C13 . C14 . 116.4(4) yes O1 . C13 . C14 . 122.1(4) yes C13 . C14 . C15 . 117.9(4) yes C13 . C14 . C18 . 121.3(4) yes C15 . C14 . C18 . 120.6(4) yes C14 . C15 . C16 . 125.3(4) yes C14 . C15 . H151 . 116.9 no C16 . C15 . H151 . 117.8 no C15 . C16 . C17 . 116.0(4) yes C15 . C16 . C22 . 119.9(4) yes C17 . C16 . C22 . 124.1(4) yes C12 . C17 . C16 . 121.9(4) yes C12 . C17 . H171 . 119.0 no C16 . C17 . H171 . 119.1 no C14 . C18 . C19 . 111.7(4) yes C14 . C18 . C20 . 109.0(4) yes C19 . C18 . C20 . 109.2(4) yes C14 . C18 . C21 . 111.9(4) yes C19 . C18 . C21 . 106.9(4) yes C20 . C18 . C21 . 108.0(4) yes C18 . C19 . H191 . 109.3 no C18 . C19 . H192 . 109.5 no H191 . C19 . H192 . 109.5 no C18 . C19 . H193 . 109.7 no H191 . C19 . H193 . 109.5 no H192 . C19 . H193 . 109.5 no C18 . C20 . H201 . 109.5 no C18 . C20 . H202 . 110.0 no H201 . C20 . H202 . 109.5 no C18 . C20 . H203 . 108.9 no H201 . C20 . H203 . 109.5 no H202 . C20 . H203 . 109.5 no C18 . C21 . H211 . 109.6 no C18 . C21 . H212 . 109.7 no H211 . C21 . H212 . 109.5 no C18 . C21 . H213 . 109.1 no H211 . C21 . H213 . 109.5 no H212 . C21 . H213 . 109.5 no C16 . C22 . C23 . 109.8(4) yes C16 . C22 . C24 . 110.6(5) yes C23 . C22 . C24 . 108.7(5) yes C16 . C22 . C25 . 111.3(4) yes C23 . C22 . C25 . 109.2(6) yes C24 . C22 . C25 . 107.1(5) yes C22 . C23 . H231 . 109.6 no C22 . C23 . H232 . 109.1 no H231 . C23 . H232 . 109.5 no C22 . C23 . H233 . 109.6 no H231 . C23 . H233 . 109.5 no H232 . C23 . H233 . 109.5 no C22 . C24 . H241 . 111.1 no C22 . C24 . H242 . 109.3 no H241 . C24 . H242 . 109.5 no C22 . C24 . H243 . 108.0 no H241 . C24 . H243 . 109.5 no H242 . C24 . H243 . 109.5 no C22 . C25 . H251 . 109.9 no C22 . C25 . H252 . 110.2 no H251 . C25 . H252 . 109.5 no C22 . C25 . H253 . 108.4 no H251 . C25 . H253 . 109.5 no H252 . C25 . H253 . 109.5 no N5 . C26 . C27 . 110.8(4) yes N5 . C26 . C29 . 121.6(4) yes C27 . C26 . C29 . 127.5(5) yes C26 . C27 . C28 . 106.6(4) yes C26 . C27 . H271 . 127.1 no C28 . C27 . H271 . 126.3 no C27 . C28 . N6 . 105.9(4) yes C27 . C28 . C30 . 131.4(5) yes N6 . C28 . C30 . 122.7(5) yes C26 . C29 . H291 . 109.7 no C26 . C29 . H292 . 109.2 no H291 . C29 . H292 . 109.5 no C26 . C29 . H293 . 109.5 no H291 . C29 . H293 . 109.5 no H292 . C29 . H293 . 109.5 no C28 . C30 . H301 . 109.1 no C28 . C30 . H302 . 110.2 no H301 . C30 . H302 . 109.5 no C28 . C30 . H303 . 109.1 no H301 . C30 . H303 . 109.5 no H302 . C30 . H303 . 109.5 no N7 . C31 . C32 . 110.6(4) yes N7 . C31 . C34 . 123.7(4) yes C32 . C31 . C34 . 125.6(4) yes C31 . C32 . C33 . 107.5(4) yes C31 . C32 . H321 . 126.3 no C33 . C32 . H321 . 126.2 no C32 . C33 . N8 . 105.3(4) yes C32 . C33 . C35 . 131.1(5) yes N8 . C33 . C35 . 123.6(4) yes C31 . C34 . H341 . 110.1 no C31 . C34 . H342 . 110.5 no H341 . C34 . H342 . 109.5 no C31 . C34 . H343 . 108.9 no H341 . C34 . H343 . 108.9 no H342 . C34 . H343 . 108.9 no C33 . C35 . H351 . 109.9 no C33 . C35 . H352 . 109.3 no H351 . C35 . H352 . 109.5 no C33 . C35 . H353 . 109.2 no H351 . C35 . H353 . 109.5 no H352 . C35 . H353 . 109.5 no N6 . C36 . N8 . 110.9(3) yes N6 . C36 . C37 . 117.4(4) yes N8 . C36 . C37 . 114.8(4) yes N6 . C36 . H361 . 103.9 no N8 . C36 . H361 . 103.9 no C37 . C36 . H361 . 104.0 no C36 . C37 . C38 . 123.0(4) yes C36 . C37 . C42 . 115.0(4) yes C38 . C37 . C42 . 122.0(4) yes C37 . C38 . O2 . 121.8(4) yes C37 . C38 . C39 . 116.2(4) yes O2 . C38 . C39 . 121.9(4) yes C38 . C39 . C40 . 118.3(4) yes C38 . C39 . C43 . 120.5(4) yes C40 . C39 . C43 . 121.2(4) yes C39 . C40 . C41 . 125.7(4) yes C39 . C40 . H401 . 117.2 no C41 . C40 . H401 . 117.1 no C40 . C41 . C42 . 115.3(4) yes C40 . C41 . C47 . 123.8(4) yes C42 . C41 . C47 . 120.9(4) yes C41 . C42 . C37 . 122.2(4) yes C41 . C42 . H421 . 118.8 no C37 . C42 . H421 . 119.0 no C39 . C43 . C44 . 110.8(4) yes C39 . C43 . C45 . 111.6(4) yes C44 . C43 . C45 . 108.3(4) yes C39 . C43 . C46 . 108.8(4) yes C44 . C43 . C46 . 109.3(4) yes C45 . C43 . C46 . 108.0(4) yes C43 . C44 . H441 . 109.0 no C43 . C44 . H442 . 109.6 no H441 . C44 . H442 . 109.5 no C43 . C44 . H443 . 109.7 no H441 . C44 . H443 . 109.5 no H442 . C44 . H443 . 109.5 no C43 . C45 . H451 . 109.4 no C43 . C45 . H452 . 110.3 no H451 . C45 . H452 . 109.5 no C43 . C45 . H453 . 108.7 no H451 . C45 . H453 . 109.5 no H452 . C45 . H453 . 109.5 no C43 . C46 . H461 . 109.5 no C43 . C46 . H462 . 110.0 no H461 . C46 . H462 . 109.5 no C43 . C46 . H463 . 108.9 no H461 . C46 . H463 . 109.5 no H462 . C46 . H463 . 109.5 no C41 . C47 . C48 . 110.4(5) yes C41 . C47 . C49 . 109.7(5) yes C48 . C47 . C49 . 108.1(6) yes C41 . C47 . C50 . 112.3(5) yes C48 . C47 . C50 . 106.4(5) yes C49 . C47 . C50 . 109.8(6) yes C47 . C48 . H481 . 109.8 no C47 . C48 . H482 . 109.9 no H481 . C48 . H482 . 109.5 no C47 . C48 . H483 . 108.7 no H481 . C48 . H483 . 109.5 no H482 . C48 . H483 . 109.5 no C47 . C49 . H491 . 109.2 no C47 . C49 . H492 . 109.6 no H491 . C49 . H492 . 109.5 no C47 . C49 . H493 . 109.6 no H491 . C49 . H493 . 109.5 no H492 . C49 . H493 . 109.5 no C47 . C50 . H501 . 108.9 no C47 . C50 . H502 . 111.6 no H501 . C50 . H502 . 109.5 no C47 . C50 . H503 . 107.9 no H501 . C50 . H503 . 109.5 no H502 . C50 . H503 . 109.5 no C52 . C51 . H511 . 108.2 no C52 . C51 . H512 . 109.9 no H511 . C51 . H512 . 109.5 no C52 . C51 . H513 . 110.3 no H511 . C51 . H513 . 109.5 no H512 . C51 . H513 . 109.5 no C51 . C52 . O3 . 108.5(8) yes C51 . C52 . H521 . 110.5 no O3 . C52 . H521 . 109.2 no C51 . C52 . H522 . 110.1 no O3 . C52 . H522 . 109.0 no H521 . C52 . H522 . 109.5 no O3 . C53 . C54 . 112.4(6) yes O3 . C53 . H531 . 107.3 no C54 . C53 . H531 . 109.1 no O3 . C53 . H532 . 108.1 no C54 . C53 . H532 . 109.8 no H531 . C53 . H532 . 110.1 no C53 . C54 . H541 . 107.5 no C53 . C54 . H542 . 110.7 no H541 . C54 . H542 . 109.5 no C53 . C54 . H543 . 110.2 no H541 . C54 . H543 . 109.5 no H542 . C54 . H543 . 109.5 no _chemical_name_common 'Mg((Me2pz)2C(C6H2(tBu)2O)2 . OEt2' #===end data_compound_6.0.5(C7H8) _database_code_depnum_ccdc_archive 'CCDC 696840' # Local code ADS36 _chemical_name_systematic ; Mg{(Me2pz)2C(C6H2(tBu)2O}{N(SiMe3)2} ; _publ_section_exptl_prep ; Crystals of ADS36 contain toluene molecules of crystallization disordered over crystallographic inversion centers. These were refined isotropically with a common displacement parameter for the carbon atoms. Geometric restraints were applied to the C---C distances and C---C---C angles. H atoms were placed geometrically and refined in a riding model. The largest peak in the final Fourier difference map was in the region of the disordered toluene molecule. ; _chemical_melting_point ? _cell_length_a 11.5864(2) _cell_length_b 12.7632(2) _cell_length_c 14.2935(3) _cell_angle_alpha 105.6153(10) _cell_angle_beta 104.8024(9) _cell_angle_gamma 95.2213(10) _cell_volume 1938.95(6) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Si 0.0817 0.0704 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Mg 0.0486 0.0363 5.4204 2.8275 2.1735 79.2611 1.2269 0.3808 2.3073 7.1937 0.8584 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 _chemical_formula_sum 'C34.50 H57 Mg1 N5 O1 Si2' _chemical_formula_moiety 'C31 H53 Mg1 N5 O1 Si2, 0.5(C7 H8)' _chemical_compound_source ? _chemical_formula_weight 638.34 _cell_measurement_reflns_used 7897 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.093 _exptl_crystal_density_meas ? _exptl_crystal_F_000 694 _exptl_absorpt_coefficient_mu 0.139 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.97 _exptl_absorpt_correction_T_max 0.99 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 15046 _reflns_number_total 8798 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_theta_min 5.148 _diffrn_reflns_theta_max 27.480 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.106 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _reflns_limit_h_min -15 _reflns_limit_h_max 14 _reflns_limit_k_min -16 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _oxford_diffrn_Wilson_B_factor 2.68 _oxford_diffrn_Wilson_scale 4.86 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.69 _refine_diff_density_max 1.55 _refine_ls_number_reflns 4887 _refine_ls_number_restraints 21 _refine_ls_number_parameters 380 _refine_ls_wR_factor_ref 0.0704 _refine_ls_goodness_of_fit_ref 1.1222 _refine_ls_R_factor_all 0.1156 _refine_ls_wR_factor_all 0.1027 _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 4887 _refine_ls_R_factor_gt 0.0642 _refine_ls_wR_factor_gt 0.0704 _refine_ls_shift/su_max 0.009587 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.912 0.331 0.594 0.149E-02 0.141 ; 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Mg1 Mg 1.05953(9) 1.20851(8) 0.78551(7) 0.0250 1.0000 Uani . . . . . . O1 O 0.89891(18) 1.13842(17) 0.76455(16) 0.0294 1.0000 Uani . . . . . . N1 N 1.1274(2) 1.1396(2) 0.90202(18) 0.0277 1.0000 Uani . . . . . . N2 N 1.1002(2) 1.0277(2) 0.87860(17) 0.0249 1.0000 Uani . . . . . . N3 N 1.1027(2) 1.0758(2) 0.68132(18) 0.0269 1.0000 Uani . . . . . . N4 N 1.1014(2) 0.9777(2) 0.70406(18) 0.0246 1.0000 Uani . . . . . . N5 N 1.1155(3) 1.3651(2) 0.7973(2) 0.0338 1.0000 Uani . . . . . . Si1 Si 1.00474(10) 1.43973(8) 0.76636(8) 0.0428 1.0000 Uani . . . . . . Si2 Si 1.26555(10) 1.41364(8) 0.82735(9) 0.0464 1.0000 Uani . . . . . . C1 C 1.1809(3) 1.1765(3) 1.0025(2) 0.0323 1.0000 Uani . . . . . . C2 C 1.1880(3) 1.0886(3) 1.0428(2) 0.0362 1.0000 Uani . . . . . . C3 C 1.1364(3) 0.9948(3) 0.9634(2) 0.0307 1.0000 Uani . . . . . . C4 C 1.2198(4) 1.2983(3) 1.0548(3) 0.0486 1.0000 Uani . . . . . . C5 C 1.1180(4) 0.8770(3) 0.9613(3) 0.0416 1.0000 Uani . . . . . . C6 C 1.1464(3) 1.0601(3) 0.6015(2) 0.0319 1.0000 Uani . . . . . . C7 C 1.1723(3) 0.9536(3) 0.5733(3) 0.0369 1.0000 Uani . . . . . . C8 C 1.1423(3) 0.9023(3) 0.6383(2) 0.0323 1.0000 Uani . . . . . . C9 C 1.1632(4) 1.1499(3) 0.5557(3) 0.0442 1.0000 Uani . . . . . . C10 C 1.1484(4) 0.7870(3) 0.6434(3) 0.0518 1.0000 Uani . . . . . . C11 C 1.0384(3) 0.9550(2) 0.7752(2) 0.0240 1.0000 Uani . . . . . . C12 C 0.9012(3) 0.9458(2) 0.7374(2) 0.0247 1.0000 Uani . . . . . . C13 C 0.8404(3) 1.0363(2) 0.7350(2) 0.0256 1.0000 Uani . . . . . . C14 C 0.7103(3) 1.0132(3) 0.7005(2) 0.0295 1.0000 Uani . . . . . . C15 C 0.6529(3) 0.9037(3) 0.6642(2) 0.0323 1.0000 Uani . . . . . . C16 C 0.7129(3) 0.8134(3) 0.6614(2) 0.0311 1.0000 Uani . . . . . . C17 C 0.8373(3) 0.8370(2) 0.7007(2) 0.0275 1.0000 Uani . . . . . . C18 C 0.6372(3) 1.1084(3) 0.7043(3) 0.0370 1.0000 Uani . . . . . . C19 C 0.6646(3) 1.1793(3) 0.8158(3) 0.0435 1.0000 Uani . . . . . . C20 C 0.6678(3) 1.1786(3) 0.6400(3) 0.0426 1.0000 Uani . . . . . . C21 C 0.4997(3) 1.0669(3) 0.6644(3) 0.0505 1.0000 Uani . . . . . . C22 C 0.6392(3) 0.6954(3) 0.6161(3) 0.0372 1.0000 Uani . . . . . . C23 C 0.5703(4) 0.6780(3) 0.5052(3) 0.0531 1.0000 Uani . . . . . . C24 C 0.5492(4) 0.6793(4) 0.6740(3) 0.0634 1.0000 Uani . . . . . . C25 C 0.7210(4) 0.6089(3) 0.6196(4) 0.0637 1.0000 Uani . . . . . . C26 C 0.8882(4) 1.4271(3) 0.8330(3) 0.0563 1.0000 Uani . . . . . . C27 C 0.9284(5) 1.3887(4) 0.6258(4) 0.0728 1.0000 Uani . . . . . . C28 C 1.0582(5) 1.5928(3) 0.8005(5) 0.0767 1.0000 Uani . . . . . . C29 C 1.3075(6) 1.4685(4) 0.7283(5) 0.0879 1.0000 Uani . . . . . . C30 C 1.3533(3) 1.2992(3) 0.8388(4) 0.0604 1.0000 Uani . . . . . . C31 C 1.3269(4) 1.5287(4) 0.9503(4) 0.0659 1.0000 Uani . . . . . . C101 C 0.5000 0.0000 0.0000 0.160(3) 1.0000 Uiso DS . . . . . C102 C 0.4820(9) 0.0980(6) -0.0224(8) 0.160(3) 0.5000 Uiso D . . . . . C103 C 0.5270(10) 0.1981(6) 0.0542(12) 0.160(3) 0.5000 Uiso D . . . . . C104 C 0.5901(10) 0.1989(10) 0.1512(10) 0.160(3) 0.5000 Uiso D . . . . . C105 C 0.6080(8) 0.1003(12) 0.1740(6) 0.160(3) 0.5000 Uiso D . . . . . C106 C 0.5645(8) 0.0004(9) 0.0968(5) 0.160(3) 0.5000 Uiso D . . . . . C107 C 0.4530(8) -0.1097(6) -0.0840(7) 0.160(3) 0.5000 Uiso D . . . . . H21 H 1.2237 1.0933 1.1156 0.0397 1.0000 Uiso R . . . . . H41 H 1.3102 1.3171 1.0806 0.0830 1.0000 Uiso R . . . . . H42 H 1.1840 1.3186 1.1125 0.0875 1.0000 Uiso R . . . . . H43 H 1.1881 1.3388 1.0053 0.0755 1.0000 Uiso R . . . . . H51 H 1.1519 0.8722 1.0315 0.0895 1.0000 Uiso R . . . . . H52 H 1.1601 0.8333 0.9151 0.0816 1.0000 Uiso R . . . . . H53 H 1.0293 0.8465 0.9361 0.0748 1.0000 Uiso R . . . . . H71 H 1.2061 0.9209 0.5163 0.0518 1.0000 Uiso R . . . . . H91 H 1.1342 1.2160 0.5921 0.1008 1.0000 Uiso R . . . . . H92 H 1.2509 1.1698 0.5617 0.1066 1.0000 Uiso R . . . . . H93 H 1.1151 1.1241 0.4824 0.0898 1.0000 Uiso R . . . . . H101 H 1.1809 0.7461 0.5884 0.0673 1.0000 Uiso R . . . . . H102 H 1.2035 0.7904 0.7110 0.0794 1.0000 Uiso R . . . . . H103 H 1.0658 0.7478 0.6347 0.0818 1.0000 Uiso R . . . . . H111 H 1.0515 0.8792 0.7773 0.0205 1.0000 Uiso R . . . . . H151 H 0.5624 0.8885 0.6384 0.0344 1.0000 Uiso R . . . . . H171 H 0.8837 0.7749 0.7031 0.0296 1.0000 Uiso R . . . . . H191 H 0.6175 1.2414 0.8193 0.0575 1.0000 Uiso R . . . . . H192 H 0.7532 1.2098 0.8441 0.0343 1.0000 Uiso R . . . . . H193 H 0.6409 1.1327 0.8562 0.0481 1.0000 Uiso R . . . . . H201 H 0.6190 1.2396 0.6438 0.0727 1.0000 Uiso R . . . . . H202 H 0.7561 1.2109 0.6666 0.0583 1.0000 Uiso R . . . . . H203 H 0.6488 1.1317 0.5678 0.0560 1.0000 Uiso R . . . . . H211 H 0.4559 1.1311 0.6682 0.0616 1.0000 Uiso R . . . . . H212 H 0.4764 1.0235 0.7075 0.0517 1.0000 Uiso R . . . . . H213 H 0.4775 1.0185 0.5924 0.0599 1.0000 Uiso R . . . . . H231 H 0.5224 0.6015 0.4750 0.0687 1.0000 Uiso R . . . . . H232 H 0.6286 0.6886 0.4663 0.0791 1.0000 Uiso R . . . . . H233 H 0.5140 0.7328 0.5020 0.0889 1.0000 Uiso R . . . . . H241 H 0.5017 0.6027 0.6442 0.0869 1.0000 Uiso R . . . . . H242 H 0.5934 0.6918 0.7471 0.1195 1.0000 Uiso R . . . . . H243 H 0.4929 0.7338 0.6687 0.1119 1.0000 Uiso R . . . . . H251 H 0.6706 0.5335 0.5893 0.0759 1.0000 Uiso R . . . . . H252 H 0.7664 0.6193 0.6920 0.0847 1.0000 Uiso R . . . . . H253 H 0.7798 0.6172 0.5805 0.0677 1.0000 Uiso R . . . . . H261 H 0.8245 1.4715 0.8135 0.0931 1.0000 Uiso R . . . . . H262 H 0.9275 1.4551 0.9080 0.0915 1.0000 Uiso R . . . . . H263 H 0.8502 1.3478 0.8135 0.0990 1.0000 Uiso R . . . . . H271 H 0.8634 1.4326 0.6080 0.1245 1.0000 Uiso R . . . . . H272 H 0.9900 1.3982 0.5896 0.1065 1.0000 Uiso R . . . . . H273 H 0.8918 1.3089 0.6049 0.0888 1.0000 Uiso R . . . . . H281 H 0.9876 1.6296 0.7798 0.1021 1.0000 Uiso R . . . . . H282 H 1.0965 1.6234 0.8756 0.1319 1.0000 Uiso R . . . . . H283 H 1.1189 1.6065 0.7646 0.0972 1.0000 Uiso R . . . . . H291 H 1.3968 1.4959 0.7505 0.1308 1.0000 Uiso R . . . . . H292 H 1.2632 1.5306 0.7201 0.1171 1.0000 Uiso R . . . . . H293 H 1.2848 1.4083 0.6620 0.1944 1.0000 Uiso R . . . . . H301 H 1.4417 1.3283 0.8566 0.1038 1.0000 Uiso R . . . . . H302 H 1.3374 1.2695 0.8932 0.1049 1.0000 Uiso R . . . . . H303 H 1.3279 1.2388 0.7726 0.0892 1.0000 Uiso R . . . . . H311 H 1.4155 1.5532 0.9631 0.1070 1.0000 Uiso R . . . . . H312 H 1.2834 1.5922 0.9466 0.1048 1.0000 Uiso R . . . . . H313 H 1.3140 1.5015 1.0070 0.1184 1.0000 Uiso R . . . . . H1071 H 0.4096 -0.0955 -0.1483 0.1727 0.5000 Uiso R . . . . . H1072 H 0.5225 -0.1478 -0.0945 0.1727 0.5000 Uiso R . . . . . H1073 H 0.3959 -0.1575 -0.0646 0.1727 0.5000 Uiso R . . . . . H1021 H 0.4371 0.0966 -0.0926 0.1727 0.5000 Uiso R . . . . . H1061 H 0.5789 -0.0709 0.1105 0.1727 0.5000 Uiso R . . . . . H1051 H 0.6513 0.1018 0.2446 0.1727 0.5000 Uiso R . . . . . H1041 H 0.6228 0.2708 0.2063 0.1727 0.5000 Uiso R . . . . . H1031 H 0.5152 0.2695 0.0397 0.1727 0.5000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0262(5) 0.0211(5) 0.0271(5) 0.0074(4) 0.0069(4) 0.0028(4) O1 0.0255(11) 0.0231(10) 0.0372(12) 0.0056(9) 0.0087(9) 0.0044(8) N1 0.0326(13) 0.0232(12) 0.0233(12) 0.0034(10) 0.0062(10) 0.0024(10) N2 0.0275(12) 0.0253(12) 0.0211(12) 0.0071(10) 0.0057(10) 0.0046(10) N3 0.0298(13) 0.0261(13) 0.0261(12) 0.0092(10) 0.0098(10) 0.0030(10) N4 0.0276(12) 0.0249(12) 0.0226(12) 0.0069(10) 0.0088(10) 0.0065(10) N5 0.0391(15) 0.0248(13) 0.0358(14) 0.0078(11) 0.0103(12) 0.0038(11) Si1 0.0531(6) 0.0246(5) 0.0460(6) 0.0114(4) 0.0049(5) 0.0077(4) Si2 0.0432(6) 0.0301(5) 0.0613(7) 0.0013(5) 0.0244(5) -0.0043(4) C1 0.0364(17) 0.0323(17) 0.0239(14) 0.0036(13) 0.0058(13) 0.0075(13) C2 0.0438(19) 0.0414(19) 0.0220(14) 0.0096(14) 0.0063(14) 0.0107(15) C3 0.0319(16) 0.0355(17) 0.0267(15) 0.0125(13) 0.0078(13) 0.0078(13) C4 0.064(3) 0.0361(19) 0.0319(17) -0.0028(15) 0.0048(17) 0.0067(17) C5 0.057(2) 0.0384(19) 0.0349(18) 0.0211(15) 0.0109(16) 0.0108(16) C6 0.0290(16) 0.0407(18) 0.0220(14) 0.0060(13) 0.0071(12) -0.0020(13) C7 0.0352(17) 0.0431(19) 0.0316(16) 0.0037(14) 0.0166(14) 0.0061(14) C8 0.0324(16) 0.0322(17) 0.0302(16) 0.0034(13) 0.0099(13) 0.0112(13) C9 0.050(2) 0.050(2) 0.0381(18) 0.0184(17) 0.0198(16) 0.0004(17) C10 0.075(3) 0.038(2) 0.051(2) 0.0103(17) 0.030(2) 0.0279(19) C11 0.0255(14) 0.0239(14) 0.0211(13) 0.0059(11) 0.0050(11) 0.0041(11) C12 0.0252(14) 0.0266(15) 0.0204(13) 0.0060(11) 0.0058(11) 0.0016(11) C13 0.0255(14) 0.0275(15) 0.0231(14) 0.0072(12) 0.0072(12) 0.0023(11) C14 0.0258(15) 0.0328(16) 0.0250(14) 0.0033(13) 0.0055(12) 0.0029(12) C15 0.0243(15) 0.0402(18) 0.0266(15) 0.0048(13) 0.0057(12) -0.0024(13) C16 0.0321(16) 0.0312(16) 0.0254(15) 0.0078(13) 0.0050(12) -0.0045(13) C17 0.0351(16) 0.0241(15) 0.0245(14) 0.0098(12) 0.0090(12) 0.0021(12) C18 0.0243(15) 0.0434(19) 0.0332(17) -0.0023(14) 0.0048(13) 0.0092(13) C19 0.0336(18) 0.049(2) 0.0384(19) -0.0003(16) 0.0078(15) 0.0114(15) C20 0.0406(19) 0.041(2) 0.0400(19) 0.0086(16) 0.0022(15) 0.0160(15) C21 0.0277(18) 0.057(2) 0.054(2) -0.0011(19) 0.0069(16) 0.0121(16) C22 0.0375(18) 0.0333(17) 0.0324(17) 0.0085(14) 0.0020(14) -0.0079(14) C23 0.064(3) 0.042(2) 0.0357(19) 0.0046(17) -0.0006(18) -0.0136(18) C24 0.063(3) 0.061(3) 0.057(3) 0.015(2) 0.017(2) -0.021(2) C25 0.051(2) 0.031(2) 0.086(3) 0.011(2) -0.007(2) -0.0056(17) C26 0.054(2) 0.041(2) 0.065(3) 0.0012(19) 0.012(2) 0.0191(18) C27 0.091(4) 0.067(3) 0.050(2) 0.018(2) -0.001(2) 0.023(3) C28 0.084(3) 0.032(2) 0.111(4) 0.030(3) 0.012(3) 0.016(2) C29 0.115(5) 0.052(3) 0.109(4) 0.013(3) 0.076(4) -0.011(3) C30 0.0314(19) 0.047(2) 0.088(3) -0.004(2) 0.021(2) 0.0028(16) C31 0.047(2) 0.041(2) 0.086(3) -0.008(2) 0.011(2) -0.0028(18) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.4686(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mg1 . O1 . 1.903(2) yes Mg1 . N1 . 2.100(3) yes Mg1 . N3 . 2.124(3) yes Mg1 . N5 . 1.992(3) yes O1 . C13 . 1.316(4) yes N1 . N2 . 1.363(3) yes N1 . C1 . 1.341(4) yes N2 . C3 . 1.366(4) yes N2 . C11 . 1.469(3) yes N3 . N4 . 1.376(3) yes N3 . C6 . 1.338(4) yes N4 . C8 . 1.362(4) yes N4 . C11 . 1.466(4) yes N5 . Si1 . 1.705(3) yes N5 . Si2 . 1.694(3) yes Si1 . C26 . 1.859(5) yes Si1 . C27 . 1.877(5) yes Si1 . C28 . 1.884(4) yes Si2 . C29 . 1.885(5) yes Si2 . C30 . 1.873(4) yes Si2 . C31 . 1.880(4) yes C1 . C2 . 1.391(5) yes C1 . C4 . 1.501(5) yes C2 . C3 . 1.368(4) yes C2 . H21 . 1.000 no C3 . C5 . 1.491(5) yes C4 . H41 . 1.000 no C4 . H42 . 1.000 no C4 . H43 . 1.000 no C5 . H51 . 1.000 no C5 . H52 . 1.000 no C5 . H53 . 1.000 no C6 . C7 . 1.393(5) yes C6 . C9 . 1.486(5) yes C7 . C8 . 1.366(5) yes C7 . H71 . 1.000 no C8 . C10 . 1.500(5) yes C9 . H91 . 1.000 no C9 . H92 . 1.000 no C9 . H93 . 1.000 no C10 . H101 . 1.000 no C10 . H102 . 1.000 no C10 . H103 . 1.000 no C11 . C12 . 1.526(4) yes C11 . H111 . 1.000 no C12 . C13 . 1.411(4) yes C12 . C17 . 1.404(4) yes C13 . C14 . 1.437(4) yes C14 . C15 . 1.388(4) yes C14 . C18 . 1.540(5) yes C15 . C16 . 1.397(5) yes C15 . H151 . 1.000 no C16 . C17 . 1.379(4) yes C16 . C22 . 1.540(4) yes C17 . H171 . 1.000 no C18 . C19 . 1.540(5) yes C18 . C20 . 1.525(5) yes C18 . C21 . 1.537(5) yes C19 . H191 . 1.000 no C19 . H192 . 1.000 no C19 . H193 . 1.000 no C20 . H201 . 1.000 no C20 . H202 . 1.000 no C20 . H203 . 1.000 no C21 . H211 . 1.000 no C21 . H212 . 1.000 no C21 . H213 . 1.000 no C22 . C23 . 1.527(5) yes C22 . C24 . 1.519(5) yes C22 . C25 . 1.522(6) yes C23 . H231 . 1.000 no C23 . H232 . 1.000 no C23 . H233 . 1.000 no C24 . H241 . 1.000 no C24 . H242 . 1.000 no C24 . H243 . 1.000 no C25 . H251 . 1.000 no C25 . H252 . 1.000 no C25 . H253 . 1.000 no C26 . H261 . 1.000 no C26 . H262 . 1.000 no C26 . H263 . 1.000 no C27 . H271 . 1.000 no C27 . H272 . 1.000 no C27 . H273 . 1.000 no C28 . H281 . 1.000 no C28 . H282 . 1.000 no C28 . H283 . 1.000 no C29 . H291 . 1.000 no C29 . H292 . 1.000 no C29 . H293 . 1.000 no C30 . H301 . 1.000 no C30 . H302 . 1.000 no C30 . H303 . 1.000 no C31 . H311 . 1.000 no C31 . H312 . 1.000 no C31 . H313 . 1.000 no C101 . C107 2_655 1.523(5) yes C101 . C106 2_655 1.393(5) yes C101 . C102 2_655 1.392(5) yes C101 . C102 . 1.392(5) yes C101 . C106 . 1.393(5) yes C101 . C107 . 1.523(5) yes C102 . C103 . 1.392(5) yes C102 . H1021 . 1.000 no C103 . C104 . 1.390(5) yes C103 . H1031 . 1.000 no C104 . C105 . 1.402(5) yes C104 . H1041 . 1.000 no C105 . C106 . 1.393(5) yes C105 . H1051 . 1.000 no C106 . H1061 . 1.000 no C107 . H1071 . 1.000 no C107 . H1072 . 1.000 no C107 . H1073 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . Mg1 . N1 . 91.13(10) yes O1 . Mg1 . N3 . 95.39(10) yes N1 . Mg1 . N3 . 89.26(10) yes O1 . Mg1 . N5 . 127.76(11) yes N1 . Mg1 . N5 . 122.10(11) yes N3 . Mg1 . N5 . 121.33(11) yes Mg1 . O1 . C13 . 136.54(19) yes Mg1 . N1 . N2 . 116.79(17) yes Mg1 . N1 . C1 . 137.0(2) yes N2 . N1 . C1 . 105.6(2) yes N1 . N2 . C3 . 110.9(2) yes N1 . N2 . C11 . 123.1(2) yes C3 . N2 . C11 . 126.0(2) yes Mg1 . N3 . N4 . 116.06(17) yes Mg1 . N3 . C6 . 138.1(2) yes N4 . N3 . C6 . 105.2(2) yes N3 . N4 . C8 . 110.9(2) yes N3 . N4 . C11 . 121.5(2) yes C8 . N4 . C11 . 126.3(3) yes Mg1 . N5 . Si1 . 116.15(15) yes Mg1 . N5 . Si2 . 119.84(15) yes Si1 . N5 . Si2 . 123.82(16) yes N5 . Si1 . C26 . 111.29(17) yes N5 . Si1 . C27 . 109.79(19) yes C26 . Si1 . C27 . 108.4(2) yes N5 . Si1 . C28 . 115.08(19) yes C26 . Si1 . C28 . 104.9(2) yes C27 . Si1 . C28 . 107.0(2) yes N5 . Si2 . C29 . 113.3(2) yes N5 . Si2 . C30 . 109.58(16) yes C29 . Si2 . C30 . 106.5(3) yes N5 . Si2 . C31 . 114.22(18) yes C29 . Si2 . C31 . 105.7(2) yes C30 . Si2 . C31 . 107.1(2) yes N1 . C1 . C2 . 110.4(3) yes N1 . C1 . C4 . 119.7(3) yes C2 . C1 . C4 . 129.9(3) yes C1 . C2 . C3 . 106.6(3) yes C1 . C2 . H21 . 126.7 no C3 . C2 . H21 . 126.8 no C2 . C3 . N2 . 106.6(3) yes C2 . C3 . C5 . 130.4(3) yes N2 . C3 . C5 . 123.0(3) yes C1 . C4 . H41 . 110.1 no C1 . C4 . H42 . 108.1 no H41 . C4 . H42 . 110.1 no C1 . C4 . H43 . 108.8 no H41 . C4 . H43 . 110.1 no H42 . C4 . H43 . 109.5 no C3 . C5 . H51 . 109.3 no C3 . C5 . H52 . 109.8 no H51 . C5 . H52 . 109.5 no C3 . C5 . H53 . 109.2 no H51 . C5 . H53 . 109.5 no H52 . C5 . H53 . 109.5 no N3 . C6 . C7 . 110.5(3) yes N3 . C6 . C9 . 121.0(3) yes C7 . C6 . C9 . 128.4(3) yes C6 . C7 . C8 . 106.7(3) yes C6 . C7 . H71 . 126.8 no C8 . C7 . H71 . 126.5 no C7 . C8 . N4 . 106.6(3) yes C7 . C8 . C10 . 130.7(3) yes N4 . C8 . C10 . 122.7(3) yes C6 . C9 . H91 . 109.1 no C6 . C9 . H92 . 109.9 no H91 . C9 . H92 . 109.6 no C6 . C9 . H93 . 109.2 no H91 . C9 . H93 . 109.6 no H92 . C9 . H93 . 109.5 no C8 . C10 . H101 . 109.3 no C8 . C10 . H102 . 109.0 no H101 . C10 . H102 . 109.5 no C8 . C10 . H103 . 110.1 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no N2 . C11 . N4 . 110.2(2) yes N2 . C11 . C12 . 117.1(2) yes N4 . C11 . C12 . 113.7(2) yes N2 . C11 . H111 . 105.0 no N4 . C11 . H111 . 104.8 no C12 . C11 . H111 . 104.7 no C11 . C12 . C13 . 124.4(3) yes C11 . C12 . C17 . 114.3(3) yes C13 . C12 . C17 . 121.2(3) yes C12 . C13 . O1 . 122.2(3) yes C12 . C13 . C14 . 117.1(3) yes O1 . C13 . C14 . 120.6(3) yes C13 . C14 . C15 . 118.5(3) yes C13 . C14 . C18 . 120.2(3) yes C15 . C14 . C18 . 121.2(3) yes C14 . C15 . C16 . 124.5(3) yes C14 . C15 . H151 . 117.8 no C16 . C15 . H151 . 117.7 no C15 . C16 . C17 . 116.4(3) yes C15 . C16 . C22 . 119.6(3) yes C17 . C16 . C22 . 123.9(3) yes C12 . C17 . C16 . 122.0(3) yes C12 . C17 . H171 . 118.9 no C16 . C17 . H171 . 119.1 no C14 . C18 . C19 . 108.6(3) yes C14 . C18 . C20 . 111.3(3) yes C19 . C18 . C20 . 110.6(3) yes C14 . C18 . C21 . 112.4(3) yes C19 . C18 . C21 . 106.8(3) yes C20 . C18 . C21 . 107.0(3) yes C18 . C19 . H191 . 109.5 no C18 . C19 . H192 . 109.4 no H191 . C19 . H192 . 109.5 no C18 . C19 . H193 . 109.5 no H191 . C19 . H193 . 109.5 no H192 . C19 . H193 . 109.5 no C18 . C20 . H201 . 109.6 no C18 . C20 . H202 . 109.2 no H201 . C20 . H202 . 109.5 no C18 . C20 . H203 . 109.6 no H201 . C20 . H203 . 109.5 no H202 . C20 . H203 . 109.5 no C18 . C21 . H211 . 109.8 no C18 . C21 . H212 . 108.7 no H211 . C21 . H212 . 109.5 no C18 . C21 . H213 . 109.9 no H211 . C21 . H213 . 109.5 no H212 . C21 . H213 . 109.5 no C16 . C22 . C23 . 108.8(3) yes C16 . C22 . C24 . 110.3(3) yes C23 . C22 . C24 . 109.1(3) yes C16 . C22 . C25 . 111.6(3) yes C23 . C22 . C25 . 108.2(3) yes C24 . C22 . C25 . 108.8(4) yes C22 . C23 . H231 . 109.4 no C22 . C23 . H232 . 109.9 no H231 . C23 . H232 . 109.5 no C22 . C23 . H233 . 109.0 no H231 . C23 . H233 . 109.5 no H232 . C23 . H233 . 109.5 no C22 . C24 . H241 . 109.9 no C22 . C24 . H242 . 109.8 no H241 . C24 . H242 . 109.5 no C22 . C24 . H243 . 108.6 no H241 . C24 . H243 . 109.5 no H242 . C24 . H243 . 109.5 no C22 . C25 . H251 . 109.5 no C22 . C25 . H252 . 108.9 no H251 . C25 . H252 . 109.5 no C22 . C25 . H253 . 110.0 no H251 . C25 . H253 . 109.5 no H252 . C25 . H253 . 109.5 no Si1 . C26 . H261 . 109.6 no Si1 . C26 . H262 . 109.3 no H261 . C26 . H262 . 109.5 no Si1 . C26 . H263 . 109.5 no H261 . C26 . H263 . 109.5 no H262 . C26 . H263 . 109.5 no Si1 . C27 . H271 . 109.5 no Si1 . C27 . H272 . 108.8 no H271 . C27 . H272 . 109.5 no Si1 . C27 . H273 . 110.0 no H271 . C27 . H273 . 109.5 no H272 . C27 . H273 . 109.5 no Si1 . C28 . H281 . 109.5 no Si1 . C28 . H282 . 109.2 no H281 . C28 . H282 . 109.5 no Si1 . C28 . H283 . 109.6 no H281 . C28 . H283 . 109.5 no H282 . C28 . H283 . 109.5 no Si2 . C29 . H291 . 109.4 no Si2 . C29 . H292 . 109.3 no H291 . C29 . H292 . 109.5 no Si2 . C29 . H293 . 109.7 no H291 . C29 . H293 . 109.5 no H292 . C29 . H293 . 109.5 no Si2 . C30 . H301 . 109.2 no Si2 . C30 . H302 . 109.7 no H301 . C30 . H302 . 109.5 no Si2 . C30 . H303 . 109.5 no H301 . C30 . H303 . 109.5 no H302 . C30 . H303 . 109.5 no Si2 . C31 . H311 . 109.9 no Si2 . C31 . H312 . 109.4 no H311 . C31 . H312 . 109.5 no Si2 . C31 . H313 . 109.1 no H311 . C31 . H313 . 109.5 no H312 . C31 . H313 . 109.5 no C107 2_655 C101 . C106 2_655 119.18(19) yes C107 2_655 C101 . C102 2_655 119.43(19) yes C106 2_655 C101 . C102 2_655 121.3(3) yes C107 2_655 C101 . C102 . 60.57(19) yes C106 2_655 C101 . C102 . 58.7(3) yes C102 2_655 C101 . C102 . 179.992 yes C107 2_655 C101 . C106 . 60.82(19) yes C106 2_655 C101 . C106 . 179.992 yes C102 2_655 C101 . C106 . 58.7(3) yes C102 . C101 . C106 . 121.3(3) yes C107 2_655 C101 . C107 . 179.992 yes C106 2_655 C101 . C107 . 60.82(19) yes C102 2_655 C101 . C107 . 60.57(19) yes C102 . C101 . C107 . 119.43(19) yes C106 . C101 . C107 . 119.18(19) yes C101 . C102 . C103 . 119.2(5) yes C101 . C102 . H1021 . 120.5 no C103 . C102 . H1021 . 120.2 no C102 . C103 . C104 . 119.6(7) yes C102 . C103 . H1031 . 120.6 no C104 . C103 . H1031 . 119.7 no C103 . C104 . C105 . 121.2(7) yes C103 . C104 . H1041 . 119.8 no C105 . C104 . H1041 . 119.0 no C104 . C105 . C106 . 119.0(7) yes C104 . C105 . H1051 . 120.5 no C106 . C105 . H1051 . 120.6 no C105 . C106 . C101 . 119.6(5) yes C105 . C106 . H1061 . 120.5 no C101 . C106 . H1061 . 120.0 no C101 . C107 . H1071 . 109.1 no C101 . C107 . H1072 . 109.7 no H1071 . C107 . H1072 . 109.5 no C101 . C107 . H1073 . 109.6 no H1071 . C107 . H1073 . 109.5 no H1072 . C107 . H1073 . 109.5 no _chemical_name_common Mg((Me2pz)2C(C6H2(tBu)2O)(N(SiMe3)2) #===end data_compound_8 _database_code_depnum_ccdc_archive 'CCDC 696841' # Local code ADS27 _chemical_name_systematic ; Zn{(Me2pz)2C(C6H2(tBu)2O}Me ; _publ_section_exptl_refinement ; H atoms were placed geometrically against orientations determined from a Fourier map. H atoms were refined in a riding model ; _chemical_melting_point ? _cell_length_a 10.1798(2) _cell_length_b 11.0522(3) _cell_length_c 12.7119(3) _cell_angle_alpha 69.3059(11) _cell_angle_beta 85.6402(11) _cell_angle_gamma 79.8464(11) _cell_volume 1316.83(5) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Zn 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 _chemical_formula_sum 'C26 H38 N4 O1 Zn1' _chemical_formula_moiety 'C26 H38 N4 O1 Zn1' _chemical_compound_source ? _chemical_formula_weight 487.99 _cell_measurement_reflns_used 5482 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.231 _exptl_crystal_density_meas ? _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 0.956 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 0.98 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 10580 _reflns_number_total 5970 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_theta_min 5.144 _diffrn_reflns_theta_max 27.500 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.300 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min -13 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _oxford_diffrn_Wilson_B_factor 1.97 _oxford_diffrn_Wilson_scale 5.54 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.35 _refine_diff_density_max 0.33 _refine_ls_number_reflns 4148 _refine_ls_number_restraints 0 _refine_ls_number_parameters 289 _refine_ls_wR_factor_ref 0.0335 _refine_ls_goodness_of_fit_ref 1.1172 _refine_ls_R_factor_all 0.0610 _refine_ls_wR_factor_all 0.0466 _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 4148 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_gt 0.0335 _refine_ls_shift/su_max 0.000732 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.808 0.448 0.767 0.189 0.221 ; 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Zn1 Zn 0.65284(3) 0.25995(3) 0.09625(2) 0.0249 1.0000 Uani . . . . . . N1 N 0.77922(18) 0.07875(18) 0.13865(15) 0.0260 1.0000 Uani . . . . . . N2 N 0.91373(18) 0.08003(17) 0.12616(14) 0.0229 1.0000 Uani . . . . . . N3 N 0.79563(17) 0.32923(17) -0.02800(14) 0.0221 1.0000 Uani . . . . . . N4 N 0.92373(16) 0.30355(16) 0.00819(13) 0.0204 1.0000 Uani . . . . . . O1 O 0.72307(14) 0.32736(14) 0.19851(12) 0.0245 1.0000 Uani . . . . . . C1 C 0.7647(3) -0.0461(2) 0.16452(18) 0.0327 1.0000 Uani . . . . . . C2 C 0.8892(3) -0.1252(2) 0.17128(19) 0.0351 1.0000 Uani . . . . . . C3 C 0.9830(2) -0.0433(2) 0.14730(18) 0.0299 1.0000 Uani . . . . . . C4 C 0.6286(3) -0.0838(3) 0.1813(2) 0.0473 1.0000 Uani . . . . . . C5 C 1.1313(3) -0.0736(3) 0.1466(2) 0.0400 1.0000 Uani . . . . . . C6 C 0.7940(2) 0.4235(2) -0.12897(17) 0.0240 1.0000 Uani . . . . . . C7 C 0.9213(2) 0.4588(2) -0.15716(17) 0.0248 1.0000 Uani . . . . . . C8 C 1.0018(2) 0.3816(2) -0.06812(17) 0.0229 1.0000 Uani . . . . . . C9 C 0.6680(2) 0.4748(2) -0.1942(2) 0.0344 1.0000 Uani . . . . . . C10 C 1.1455(2) 0.3757(2) -0.04799(19) 0.0290 1.0000 Uani . . . . . . C11 C 0.9686(2) 0.19874(19) 0.11343(16) 0.0206 1.0000 Uani . . . . . . C12 C 0.95467(19) 0.23293(19) 0.21924(16) 0.0188 1.0000 Uani . . . . . . C13 C 0.83387(19) 0.29099(19) 0.25654(16) 0.0194 1.0000 Uani . . . . . . C14 C 0.83643(19) 0.31265(19) 0.36122(16) 0.0195 1.0000 Uani . . . . . . C15 C 0.9539(2) 0.27121(19) 0.42142(16) 0.0206 1.0000 Uani . . . . . . C16 C 1.0737(2) 0.21008(19) 0.38601(16) 0.0194 1.0000 Uani . . . . . . C17 C 1.07044(19) 0.19412(19) 0.28333(16) 0.0193 1.0000 Uani . . . . . . C18 C 0.7105(2) 0.3777(2) 0.40696(18) 0.0247 1.0000 Uani . . . . . . C19 C 0.5960(2) 0.2982(2) 0.4225(2) 0.0324 1.0000 Uani . . . . . . C20 C 0.6680(2) 0.5180(2) 0.3258(2) 0.0313 1.0000 Uani . . . . . . C21 C 0.7328(2) 0.3865(3) 0.5216(2) 0.0351 1.0000 Uani . . . . . . C22 C 1.1954(2) 0.1594(2) 0.46217(17) 0.0230 1.0000 Uani . . . . . . C23 C 1.3195(2) 0.1149(3) 0.4018(2) 0.0334 1.0000 Uani . . . . . . C24 C 1.2261(2) 0.2664(2) 0.5030(2) 0.0320 1.0000 Uani . . . . . . C25 C 1.1644(2) 0.0422(2) 0.56427(19) 0.0314 1.0000 Uani . . . . . . C26 C 0.4652(2) 0.2711(3) 0.0594(2) 0.0387 1.0000 Uani . . . . . . H21 H 0.9067 -0.2224 0.1899 0.0420 1.0000 Uiso R . . . . . H41 H 0.6233 -0.1639 0.2491 0.0609 1.0000 Uiso R . . . . . H42 H 0.5586 -0.0106 0.1874 0.0609 1.0000 Uiso R . . . . . H43 H 0.6084 -0.1038 0.1140 0.0609 1.0000 Uiso R . . . . . H51 H 1.1605 -0.1698 0.1642 0.0483 1.0000 Uiso R . . . . . H52 H 1.1668 -0.0460 0.2043 0.0483 1.0000 Uiso R . . . . . H53 H 1.1663 -0.0247 0.0705 0.0483 1.0000 Uiso R . . . . . H71 H 0.9480 0.5269 -0.2276 0.0313 1.0000 Uiso R . . . . . H91 H 0.6448 0.5701 -0.2047 0.0410 1.0000 Uiso R . . . . . H92 H 0.5971 0.4272 -0.1473 0.0410 1.0000 Uiso R . . . . . H93 H 0.6792 0.4614 -0.2683 0.0410 1.0000 Uiso R . . . . . H101 H 1.1845 0.4403 -0.1141 0.0370 1.0000 Uiso R . . . . . H102 H 1.1538 0.3974 0.0210 0.0370 1.0000 Uiso R . . . . . H103 H 1.1945 0.2855 -0.0372 0.0370 1.0000 Uiso R . . . . . H111 H 1.0669 0.1753 0.1026 0.0250 1.0000 Uiso R . . . . . H151 H 0.9537 0.2856 0.4948 0.0260 1.0000 Uiso R . . . . . H171 H 1.1539 0.1538 0.2537 0.0239 1.0000 Uiso R . . . . . H191 H 0.5149 0.3419 0.4522 0.0428 1.0000 Uiso R . . . . . H192 H 0.6234 0.2077 0.4769 0.0428 1.0000 Uiso R . . . . . H193 H 0.5755 0.2935 0.3484 0.0428 1.0000 Uiso R . . . . . H201 H 0.5859 0.5601 0.3557 0.0381 1.0000 Uiso R . . . . . H202 H 0.7418 0.5697 0.3179 0.0381 1.0000 Uiso R . . . . . H203 H 0.6491 0.5154 0.2506 0.0381 1.0000 Uiso R . . . . . H211 H 0.6485 0.4293 0.5481 0.0470 1.0000 Uiso R . . . . . H212 H 0.8052 0.4395 0.5147 0.0470 1.0000 Uiso R . . . . . H213 H 0.7595 0.2963 0.5770 0.0470 1.0000 Uiso R . . . . . H231 H 1.3966 0.0827 0.4541 0.0414 1.0000 Uiso R . . . . . H232 H 1.3403 0.1902 0.3345 0.0414 1.0000 Uiso R . . . . . H233 H 1.3028 0.0425 0.3771 0.0414 1.0000 Uiso R . . . . . H241 H 1.3059 0.2313 0.5526 0.0437 1.0000 Uiso R . . . . . H242 H 1.2451 0.3436 0.4368 0.0437 1.0000 Uiso R . . . . . H243 H 1.1477 0.2939 0.5464 0.0437 1.0000 Uiso R . . . . . H251 H 1.2430 0.0078 0.6152 0.0383 1.0000 Uiso R . . . . . H252 H 1.0847 0.0706 0.6060 0.0383 1.0000 Uiso R . . . . . H253 H 1.1455 -0.0282 0.5381 0.0383 1.0000 Uiso R . . . . . H261 H 0.4229 0.3652 0.0300 0.0509 1.0000 Uiso R . . . . . H262 H 0.4631 0.2310 0.0004 0.0509 1.0000 Uiso R . . . . . H263 H 0.4160 0.2229 0.1283 0.0509 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02205(13) 0.03083(15) 0.02503(13) -0.01277(11) -0.00228(9) -0.00529(10) N1 0.0329(10) 0.0243(9) 0.0232(9) -0.0095(7) -0.0007(7) -0.0084(8) N2 0.0299(9) 0.0208(9) 0.0187(8) -0.0081(7) -0.0032(7) -0.0017(7) N3 0.0211(8) 0.0244(9) 0.0201(8) -0.0077(7) -0.0057(7) 0.0004(7) N4 0.0205(8) 0.0222(9) 0.0184(8) -0.0074(7) -0.0032(6) -0.0010(7) O1 0.0215(7) 0.0279(8) 0.0265(7) -0.0137(6) -0.0052(6) 0.0005(6) C1 0.0535(15) 0.0271(12) 0.0216(11) -0.0102(9) -0.0006(10) -0.0136(11) C2 0.0610(16) 0.0196(11) 0.0266(11) -0.0101(9) -0.0042(11) -0.0055(11) C3 0.0471(14) 0.0228(11) 0.0193(10) -0.0111(9) -0.0058(9) 0.0059(10) C4 0.0610(18) 0.0408(15) 0.0460(15) -0.0135(12) -0.0008(13) -0.0270(13) C5 0.0498(15) 0.0325(13) 0.0363(13) -0.0186(11) -0.0103(11) 0.0153(11) C6 0.0324(11) 0.0214(10) 0.0191(10) -0.0089(8) -0.0033(8) -0.0018(9) C7 0.0335(12) 0.0207(10) 0.0199(10) -0.0070(8) 0.0009(8) -0.0043(9) C8 0.0265(10) 0.0222(10) 0.0222(10) -0.0106(8) 0.0035(8) -0.0052(8) C9 0.0369(13) 0.0339(13) 0.0284(12) -0.0069(10) -0.0120(10) 0.0014(10) C10 0.0270(11) 0.0317(12) 0.0314(11) -0.0138(10) 0.0003(9) -0.0065(9) C11 0.0225(10) 0.0193(10) 0.0186(9) -0.0060(8) -0.0030(8) 0.0000(8) C12 0.0221(10) 0.0181(9) 0.0173(9) -0.0071(8) 0.0001(7) -0.0041(8) C13 0.0200(10) 0.0175(9) 0.0215(10) -0.0071(8) -0.0017(7) -0.0038(8) C14 0.0203(10) 0.0188(10) 0.0203(10) -0.0075(8) 0.0022(7) -0.0047(8) C15 0.0246(10) 0.0205(10) 0.0188(9) -0.0084(8) 0.0004(8) -0.0061(8) C16 0.0218(10) 0.0174(10) 0.0188(9) -0.0042(8) -0.0013(8) -0.0064(8) C17 0.0193(9) 0.0188(10) 0.0197(9) -0.0068(8) -0.0005(7) -0.0020(8) C18 0.0232(10) 0.0262(11) 0.0274(11) -0.0140(9) 0.0041(8) -0.0029(8) C19 0.0246(11) 0.0377(13) 0.0388(13) -0.0173(11) 0.0090(10) -0.0105(10) C20 0.0315(12) 0.0249(11) 0.0376(13) -0.0140(10) 0.0035(10) 0.0003(9) C21 0.0340(13) 0.0440(14) 0.0335(12) -0.0251(11) 0.0064(10) -0.0008(11) C22 0.0243(10) 0.0232(10) 0.0221(10) -0.0068(8) -0.0050(8) -0.0053(8) C23 0.0227(11) 0.0430(14) 0.0335(12) -0.0132(11) -0.0071(9) -0.0005(10) C24 0.0334(12) 0.0332(12) 0.0341(12) -0.0133(10) -0.0082(10) -0.0110(10) C25 0.0382(13) 0.0277(12) 0.0258(11) -0.0029(9) -0.0091(9) -0.0082(10) C26 0.0223(11) 0.0603(17) 0.0396(14) -0.0250(13) -0.0040(10) -0.0049(11) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.4221(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn1 . N1 . 2.0954(19) yes Zn1 . N3 . 2.0935(18) yes Zn1 . O1 . 1.9416(14) yes Zn1 . C26 . 1.974(2) yes N1 . N2 . 1.368(3) yes N1 . C1 . 1.334(3) yes N2 . C3 . 1.363(3) yes N2 . C11 . 1.468(3) yes N3 . N4 . 1.364(2) yes N3 . C6 . 1.336(3) yes N4 . C8 . 1.360(3) yes N4 . C11 . 1.467(2) yes O1 . C13 . 1.317(2) yes C1 . C2 . 1.397(4) yes C1 . C4 . 1.495(4) yes C2 . C3 . 1.374(3) yes C2 . H21 . 1.000 no C3 . C5 . 1.488(4) yes C4 . H41 . 1.000 no C4 . H42 . 1.000 no C4 . H43 . 1.000 no C5 . H51 . 1.000 no C5 . H52 . 1.000 no C5 . H53 . 1.000 no C6 . C7 . 1.404(3) yes C6 . C9 . 1.492(3) yes C7 . C8 . 1.376(3) yes C7 . H71 . 1.000 no C8 . C10 . 1.490(3) yes C9 . H91 . 1.000 no C9 . H92 . 1.000 no C9 . H93 . 1.000 no C10 . H101 . 1.000 no C10 . H102 . 1.000 no C10 . H103 . 1.000 no C11 . C12 . 1.511(3) yes C11 . H111 . 1.000 no C12 . C13 . 1.413(3) yes C12 . C17 . 1.399(3) yes C13 . C14 . 1.436(3) yes C14 . C15 . 1.387(3) yes C14 . C18 . 1.535(3) yes C15 . C16 . 1.409(3) yes C15 . H151 . 1.000 no C16 . C17 . 1.381(3) yes C16 . C22 . 1.530(3) yes C17 . H171 . 1.000 no C18 . C19 . 1.540(3) yes C18 . C20 . 1.535(3) yes C18 . C21 . 1.531(3) yes C19 . H191 . 1.000 no C19 . H192 . 1.000 no C19 . H193 . 1.000 no C20 . H201 . 1.000 no C20 . H202 . 1.000 no C20 . H203 . 1.000 no C21 . H211 . 1.000 no C21 . H212 . 1.000 no C21 . H213 . 1.000 no C22 . C23 . 1.526(3) yes C22 . C24 . 1.535(3) yes C22 . C25 . 1.534(3) yes C23 . H231 . 1.000 no C23 . H232 . 1.000 no C23 . H233 . 1.000 no C24 . H241 . 1.000 no C24 . H242 . 1.000 no C24 . H243 . 1.000 no C25 . H251 . 1.000 no C25 . H252 . 1.000 no C25 . H253 . 1.000 no C26 . H261 . 1.000 no C26 . H262 . 1.000 no C26 . H263 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Zn1 . N3 . 85.89(7) yes N1 . Zn1 . O1 . 98.15(6) yes N3 . Zn1 . O1 . 92.29(6) yes N1 . Zn1 . C26 . 119.28(10) yes N3 . Zn1 . C26 . 121.95(9) yes O1 . Zn1 . C26 . 128.78(9) yes Zn1 . N1 . N2 . 117.48(13) yes Zn1 . N1 . C1 . 136.31(17) yes N2 . N1 . C1 . 105.66(19) yes N1 . N2 . C3 . 111.14(18) yes N1 . N2 . C11 . 120.83(16) yes C3 . N2 . C11 . 127.01(18) yes Zn1 . N3 . N4 . 115.56(12) yes Zn1 . N3 . C6 . 135.55(14) yes N4 . N3 . C6 . 105.84(16) yes N3 . N4 . C8 . 111.28(16) yes N3 . N4 . C11 . 122.56(16) yes C8 . N4 . C11 . 126.06(17) yes Zn1 . O1 . C13 . 132.40(12) yes N1 . C1 . C2 . 110.4(2) yes N1 . C1 . C4 . 120.4(2) yes C2 . C1 . C4 . 129.2(2) yes C1 . C2 . C3 . 106.5(2) yes C1 . C2 . H21 . 126.8 no C3 . C2 . H21 . 126.7 no C2 . C3 . N2 . 106.3(2) yes C2 . C3 . C5 . 130.4(2) yes N2 . C3 . C5 . 123.4(2) yes C1 . C4 . H41 . 112.1 no C1 . C4 . H42 . 111.6 no H41 . C4 . H42 . 109.5 no C1 . C4 . H43 . 107.9 no H41 . C4 . H43 . 107.8 no H42 . C4 . H43 . 107.8 no C3 . C5 . H51 . 109.8 no C3 . C5 . H52 . 109.4 no H51 . C5 . H52 . 109.5 no C3 . C5 . H53 . 109.2 no H51 . C5 . H53 . 109.5 no H52 . C5 . H53 . 109.5 no N3 . C6 . C7 . 110.18(18) yes N3 . C6 . C9 . 120.2(2) yes C7 . C6 . C9 . 129.6(2) yes C6 . C7 . C8 . 106.18(18) yes C6 . C7 . H71 . 126.9 no C8 . C7 . H71 . 126.9 no C7 . C8 . N4 . 106.52(18) yes C7 . C8 . C10 . 131.3(2) yes N4 . C8 . C10 . 122.18(19) yes C6 . C9 . H91 . 107.2 no C6 . C9 . H92 . 107.2 no H91 . C9 . H92 . 109.5 no C6 . C9 . H93 . 111.0 no H91 . C9 . H93 . 110.9 no H92 . C9 . H93 . 110.9 no C8 . C10 . H101 . 109.5 no C8 . C10 . H102 . 109.3 no H101 . C10 . H102 . 109.5 no C8 . C10 . H103 . 109.6 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no N2 . C11 . N4 . 110.44(15) yes N2 . C11 . C12 . 112.93(16) yes N4 . C11 . C12 . 117.30(16) yes N2 . C11 . H111 . 105.0 no N4 . C11 . H111 . 105.0 no C12 . C11 . H111 . 104.9 no C11 . C12 . C13 . 124.01(17) yes C11 . C12 . C17 . 114.37(17) yes C13 . C12 . C17 . 121.49(17) yes C12 . C13 . O1 . 122.82(17) yes C12 . C13 . C14 . 117.03(17) yes O1 . C13 . C14 . 120.13(17) yes C13 . C14 . C15 . 118.82(17) yes C13 . C14 . C18 . 120.55(17) yes C15 . C14 . C18 . 120.62(17) yes C14 . C15 . C16 . 124.32(18) yes C14 . C15 . H151 . 117.8 no C16 . C15 . H151 . 117.8 no C15 . C16 . C17 . 115.99(18) yes C15 . C16 . C22 . 120.38(17) yes C17 . C16 . C22 . 123.55(18) yes C12 . C17 . C16 . 122.30(18) yes C12 . C17 . H171 . 118.9 no C16 . C17 . H171 . 118.8 no C14 . C18 . C19 . 110.47(17) yes C14 . C18 . C20 . 109.87(17) yes C19 . C18 . C20 . 109.78(18) yes C14 . C18 . C21 . 112.25(17) yes C19 . C18 . C21 . 107.02(18) yes C20 . C18 . C21 . 107.35(18) yes C18 . C19 . H191 . 109.4 no C18 . C19 . H192 . 109.4 no H191 . C19 . H192 . 109.5 no C18 . C19 . H193 . 109.6 no H191 . C19 . H193 . 109.5 no H192 . C19 . H193 . 109.5 no C18 . C20 . H201 . 109.7 no C18 . C20 . H202 . 109.4 no H201 . C20 . H202 . 109.5 no C18 . C20 . H203 . 109.3 no H201 . C20 . H203 . 109.5 no H202 . C20 . H203 . 109.5 no C18 . C21 . H211 . 109.5 no C18 . C21 . H212 . 109.5 no H211 . C21 . H212 . 109.5 no C18 . C21 . H213 . 109.4 no H211 . C21 . H213 . 109.5 no H212 . C21 . H213 . 109.5 no C16 . C22 . C23 . 111.87(17) yes C16 . C22 . C24 . 110.67(17) yes C23 . C22 . C24 . 108.15(18) yes C16 . C22 . C25 . 108.34(17) yes C23 . C22 . C25 . 108.69(18) yes C24 . C22 . C25 . 109.08(17) yes C22 . C23 . H231 . 109.4 no C22 . C23 . H232 . 109.5 no H231 . C23 . H232 . 109.5 no C22 . C23 . H233 . 109.5 no H231 . C23 . H233 . 109.5 no H232 . C23 . H233 . 109.5 no C22 . C24 . H241 . 109.4 no C22 . C24 . H242 . 109.5 no H241 . C24 . H242 . 109.5 no C22 . C24 . H243 . 109.5 no H241 . C24 . H243 . 109.5 no H242 . C24 . H243 . 109.5 no C22 . C25 . H251 . 109.5 no C22 . C25 . H252 . 109.5 no H251 . C25 . H252 . 109.5 no C22 . C25 . H253 . 109.3 no H251 . C25 . H253 . 109.5 no H252 . C25 . H253 . 109.5 no Zn1 . C26 . H261 . 109.2 no Zn1 . C26 . H262 . 108.8 no H261 . C26 . H262 . 109.5 no Zn1 . C26 . H263 . 109.7 no H261 . C26 . H263 . 109.8 no H262 . C26 . H263 . 109.8 no _chemical_name_common Zn((Me2pz)2C(C6H2(tBu)2O)Me #===end data_compound_9.0.35(C7H8) _database_code_depnum_ccdc_archive 'CCDC 696842' # Local code ads39 _chemical_name_systematic ; Zn{(Me2pz)2C(C6H2(tBu)2O}{N(SiMe3)2}.0.35(C7H8) ; _publ_section_exptl_prep ; The crystals contain toluene molecules of crystallization disordered over crystallographic inversion centers. These were refined isotropically with a common displacement parameter for the carbon atoms. Geometric restraints were applied to the C-C distances and C-C-C angles. H atoms were placed geometrically and refined in a riding model. The largest peak in the final Fourier difference map was in the region of the disordered toluene molecule. ; _chemical_melting_point ? _cell_length_a 11.6068(2) _cell_length_b 12.6722(2) _cell_length_c 14.2523(3) _cell_angle_alpha 105.2600(8) _cell_angle_beta 104.7969(8) _cell_angle_gamma 94.9221(8) _cell_volume 1928.81(6) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Si 0.0817 0.0704 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Zn 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 _chemical_formula_sum 'C33.45 H55.80 N5 O1 Si2 Zn1' _chemical_formula_moiety 'C31 H53 N5 O1 Si2 Zn1, 0.35(C7H8)' _chemical_compound_source ? _chemical_formula_weight 665.60 _cell_measurement_reflns_used 8420 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.10 _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_meas ? _exptl_crystal_F_000 715.000 _exptl_absorpt_coefficient_mu 0.729 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 0.96 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 15008 _reflns_number_total 8788 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_theta_min 5.101 _diffrn_reflns_theta_max 27.528 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.702 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -15 _reflns_limit_h_max 14 _reflns_limit_k_min -16 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _oxford_diffrn_Wilson_B_factor 2.57 _oxford_diffrn_Wilson_scale 5.45 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.79 _refine_diff_density_max 1.16 _refine_ls_number_reflns 5976 _refine_ls_number_restraints 21 _refine_ls_number_parameters 380 _refine_ls_wR_factor_ref 0.0542 _refine_ls_goodness_of_fit_ref 1.0560 _refine_ls_R_factor_all 0.0803 _refine_ls_wR_factor_all 0.0677 _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 5976 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_gt 0.0542 _refine_ls_shift/su_max 0.008 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.819 -0.105 0.482 -0.149 0.412E-01 ; 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Zn1 Zn 1.05958(3) 1.20523(3) 0.78478(2) 0.0278 1.0000 Uani . . . . . . O1 O 0.89464(18) 1.14033(16) 0.76444(16) 0.0336 1.0000 Uani . . . . . . N1 N 1.1218(2) 1.13664(19) 0.90039(17) 0.0308 1.0000 Uani . . . . . . N2 N 1.0995(2) 1.02369(19) 0.87728(17) 0.0287 1.0000 Uani . . . . . . N3 N 1.0990(2) 1.07565(19) 0.67990(17) 0.0298 1.0000 Uani . . . . . . N4 N 1.1031(2) 0.97792(18) 0.70371(17) 0.0275 1.0000 Uani . . . . . . N5 N 1.1157(2) 1.3570(2) 0.7973(2) 0.0387 1.0000 Uani . . . . . . Si1 Si 1.00439(10) 1.43118(7) 0.76375(8) 0.0473 1.0000 Uani . . . . . . Si2 Si 1.26665(9) 1.40433(8) 0.83139(9) 0.0512 1.0000 Uani . . . . . . C1 C 1.1707(3) 1.1742(3) 1.0010(2) 0.0364 1.0000 Uani . . . . . . C2 C 1.1805(3) 1.0855(3) 1.0422(2) 0.0389 1.0000 Uani . . . . . . C3 C 1.1340(3) 0.9906(3) 0.9620(2) 0.0329 1.0000 Uani . . . . . . C4 C 1.2030(4) 1.2955(3) 1.0533(3) 0.0520 1.0000 Uani . . . . . . C5 C 1.1204(3) 0.8719(3) 0.9602(3) 0.0444 1.0000 Uani . . . . . . C6 C 1.1450(3) 1.0642(3) 0.6022(2) 0.0352 1.0000 Uani . . . . . . C7 C 1.1768(3) 0.9586(3) 0.5745(2) 0.0407 1.0000 Uani . . . . . . C8 C 1.1494(3) 0.9055(3) 0.6403(2) 0.0368 1.0000 Uani . . . . . . C9 C 1.1577(4) 1.1561(3) 0.5561(3) 0.0496 1.0000 Uani . . . . . . C10 C 1.1620(4) 0.7907(3) 0.6469(3) 0.0603 1.0000 Uani . . . . . . C11 C 1.0394(2) 0.9533(2) 0.77382(19) 0.0270 1.0000 Uani . . . . . . C12 C 0.9032(2) 0.9450(2) 0.73604(19) 0.0273 1.0000 Uani . . . . . . C13 C 0.8407(2) 1.0364(2) 0.73487(19) 0.0282 1.0000 Uani . . . . . . C14 C 0.7108(3) 1.0123(3) 0.7007(2) 0.0341 1.0000 Uani . . . . . . C15 C 0.6548(3) 0.9022(3) 0.6645(2) 0.0373 1.0000 Uani . . . . . . C16 C 0.7150(3) 0.8115(3) 0.6613(2) 0.0350 1.0000 Uani . . . . . . C17 C 0.8400(3) 0.8361(2) 0.6994(2) 0.0312 1.0000 Uani . . . . . . C18 C 0.6362(3) 1.1075(3) 0.7055(2) 0.0414 1.0000 Uani . . . . . . C19 C 0.6619(3) 1.1778(3) 0.8163(3) 0.0494 1.0000 Uani . . . . . . C20 C 0.6657(3) 1.1794(3) 0.6412(3) 0.0471 1.0000 Uani . . . . . . C21 C 0.4992(3) 1.0647(4) 0.6650(3) 0.0569 1.0000 Uani . . . . . . C22 C 0.6429(3) 0.6940(3) 0.6172(2) 0.0439 1.0000 Uani . . . . . . C23 C 0.5700(4) 0.6766(3) 0.5081(3) 0.0544 1.0000 Uani . . . . . . C24 C 0.5556(4) 0.6775(4) 0.6789(3) 0.0691 1.0000 Uani . . . . . . C25 C 0.7247(4) 0.6064(3) 0.6194(4) 0.0687 1.0000 Uani . . . . . . C26 C 0.8913(4) 1.4244(3) 0.8338(3) 0.0585 1.0000 Uani . . . . . . C27 C 0.9272(5) 1.3771(4) 0.6240(3) 0.0711 1.0000 Uani . . . . . . C28 C 1.0604(5) 1.5836(4) 0.7919(5) 0.0890 1.0000 Uani . . . . . . C29 C 1.3133(6) 1.4600(4) 0.7337(5) 0.0975 1.0000 Uani . . . . . . C30 C 1.3533(3) 1.2899(4) 0.8465(4) 0.0690 1.0000 Uani . . . . . . C31 C 1.3217(4) 1.5201(3) 0.9545(4) 0.0672 1.0000 Uani . . . . . . C101 C 0.5000 0.0000 0.0000 0.163(4) 0.7000 Uiso DS . . . . . C102 C 0.4520(9) 0.0733(9) -0.0527(9) 0.163(4) 0.3500 Uiso D . . . . . C103 C 0.4757(14) 0.1884(9) -0.0047(16) 0.163(4) 0.3500 Uiso D . . . . . C104 C 0.5498(15) 0.2298(8) 0.0961(16) 0.163(4) 0.3500 Uiso D . . . . . C105 C 0.5972(11) 0.1564(12) 0.1487(10) 0.163(4) 0.3500 Uiso D . . . . . C106 C 0.5769(7) 0.0421(11) 0.1001(4) 0.163(4) 0.3500 Uiso D . . . . . C107 C 0.4785(10) -0.1229(5) -0.0543(10) 0.163(4) 0.3500 Uiso D . . . . . H21 H 1.2143 1.0898 1.1153 0.0445 1.0000 Uiso R . . . . . H41 H 1.1649 1.3135 1.1099 0.0563 1.0000 Uiso R . . . . . H42 H 1.1698 1.3351 1.0028 0.0563 1.0000 Uiso R . . . . . H43 H 1.2928 1.3172 1.0805 0.0563 1.0000 Uiso R . . . . . H51 H 1.1515 0.8671 1.0309 0.0565 1.0000 Uiso R . . . . . H52 H 1.1674 0.8312 0.9168 0.0565 1.0000 Uiso R . . . . . H53 H 1.0331 0.8380 0.9318 0.0565 1.0000 Uiso R . . . . . H71 H 1.2119 0.9275 0.5179 0.0483 1.0000 Uiso R . . . . . H91 H 1.1937 1.1325 0.4988 0.0620 1.0000 Uiso R . . . . . H92 H 1.2114 1.2223 0.6092 0.0620 1.0000 Uiso R . . . . . H93 H 1.0763 1.1755 0.5301 0.0620 1.0000 Uiso R . . . . . H101 H 1.1981 0.7517 0.5935 0.0788 1.0000 Uiso R . . . . . H102 H 1.2160 0.7959 0.7156 0.0788 1.0000 Uiso R . . . . . H103 H 1.0808 0.7482 0.6367 0.0788 1.0000 Uiso R . . . . . H111 H 1.0525 0.8767 0.7751 0.0321 1.0000 Uiso R . . . . . H151 H 0.5645 0.8868 0.6390 0.0416 1.0000 Uiso R . . . . . H171 H 0.8865 0.7734 0.7009 0.0363 1.0000 Uiso R . . . . . H191 H 0.6136 1.2396 0.8201 0.0568 1.0000 Uiso R . . . . . H192 H 0.7499 1.2093 0.8448 0.0568 1.0000 Uiso R . . . . . H193 H 0.6392 1.1298 0.8564 0.0568 1.0000 Uiso R . . . . . H201 H 0.6163 1.2404 0.6452 0.0555 1.0000 Uiso R . . . . . H202 H 0.7535 1.2119 0.6671 0.0555 1.0000 Uiso R . . . . . H203 H 0.6466 1.1326 0.5689 0.0555 1.0000 Uiso R . . . . . H211 H 0.4544 1.1289 0.6696 0.0618 1.0000 Uiso R . . . . . H212 H 0.4758 1.0189 0.7067 0.0618 1.0000 Uiso R . . . . . H213 H 0.4785 1.0182 0.5925 0.0618 1.0000 Uiso R . . . . . H231 H 0.5233 0.5996 0.4793 0.0599 1.0000 Uiso R . . . . . H232 H 0.6255 0.6876 0.4669 0.0599 1.0000 Uiso R . . . . . H233 H 0.5128 0.7312 0.5063 0.0599 1.0000 Uiso R . . . . . H241 H 0.5083 0.6006 0.6502 0.0890 1.0000 Uiso R . . . . . H242 H 0.6025 0.6894 0.7513 0.0890 1.0000 Uiso R . . . . . H243 H 0.4990 0.7325 0.6756 0.0890 1.0000 Uiso R . . . . . H251 H 0.6747 0.5308 0.5898 0.0793 1.0000 Uiso R . . . . . H252 H 0.7718 0.6161 0.6913 0.0793 1.0000 Uiso R . . . . . H253 H 0.7816 0.6152 0.5788 0.0793 1.0000 Uiso R . . . . . H261 H 0.8273 1.4686 0.8130 0.0686 1.0000 Uiso R . . . . . H262 H 0.9320 1.4554 0.9085 0.0686 1.0000 Uiso R . . . . . H263 H 0.8538 1.3454 0.8181 0.0686 1.0000 Uiso R . . . . . H271 H 0.8624 1.4211 0.6049 0.0858 1.0000 Uiso R . . . . . H272 H 0.9873 1.3830 0.5856 0.0858 1.0000 Uiso R . . . . . H273 H 0.8906 1.2976 0.6071 0.0858 1.0000 Uiso R . . . . . H281 H 0.9911 1.6223 0.7705 0.0983 1.0000 Uiso R . . . . . H282 H 1.1005 1.6166 0.8665 0.0983 1.0000 Uiso R . . . . . H283 H 1.1200 1.5926 0.7537 0.0983 1.0000 Uiso R . . . . . H291 H 1.4025 1.4864 0.7573 0.1195 1.0000 Uiso R . . . . . H292 H 1.2701 1.5231 0.7244 0.1195 1.0000 Uiso R . . . . . H293 H 1.2919 1.3998 0.6676 0.1195 1.0000 Uiso R . . . . . H301 H 1.4417 1.3188 0.8662 0.0768 1.0000 Uiso R . . . . . H302 H 1.3348 1.2608 0.9006 0.0768 1.0000 Uiso R . . . . . H303 H 1.3302 1.2289 0.7809 0.0768 1.0000 Uiso R . . . . . H311 H 1.4106 1.5442 0.9702 0.0706 1.0000 Uiso R . . . . . H312 H 1.2788 1.5841 0.9483 0.0706 1.0000 Uiso R . . . . . H313 H 1.3051 1.4932 1.0105 0.0706 1.0000 Uiso R . . . . . H1021 H 0.4040 0.0458 -0.1259 0.1667 0.3500 Uiso R . . . . . H1031 H 0.4439 0.2418 -0.0415 0.1667 0.3500 Uiso R . . . . . H1041 H 0.5701 0.3111 0.1323 0.1667 0.3500 Uiso R . . . . . H1051 H 0.6413 0.1832 0.2229 0.1667 0.3500 Uiso R . . . . . H1061 H 0.6136 -0.0108 0.1354 0.1667 0.3500 Uiso R . . . . . H1071 H 0.5141 -0.1650 -0.0066 0.1667 0.3500 Uiso R . . . . . H1072 H 0.5173 -0.1346 -0.1105 0.1667 0.3500 Uiso R . . . . . H1073 H 0.3896 -0.1501 -0.0833 0.1667 0.3500 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02826(16) 0.02693(16) 0.02689(16) 0.00720(12) 0.00652(12) 0.00487(11) O1 0.0279(10) 0.0285(10) 0.0389(11) 0.0040(8) 0.0057(8) 0.0061(8) N1 0.0308(12) 0.0298(11) 0.0264(11) 0.0032(9) 0.0043(9) 0.0050(9) N2 0.0288(11) 0.0312(12) 0.0240(11) 0.0079(9) 0.0042(9) 0.0055(9) N3 0.0325(12) 0.0313(12) 0.0254(11) 0.0076(9) 0.0093(9) 0.0040(9) N4 0.0292(11) 0.0264(11) 0.0251(10) 0.0050(9) 0.0071(9) 0.0060(9) N5 0.0426(14) 0.0304(12) 0.0399(14) 0.0085(11) 0.0087(11) 0.0036(11) Si1 0.0573(6) 0.0288(4) 0.0490(5) 0.0116(4) 0.0033(4) 0.0083(4) Si2 0.0451(5) 0.0390(5) 0.0607(6) -0.0040(4) 0.0235(5) -0.0060(4) C1 0.0394(16) 0.0419(16) 0.0229(13) 0.0046(12) 0.0058(11) 0.0067(13) C2 0.0408(16) 0.0492(18) 0.0236(13) 0.0112(12) 0.0029(12) 0.0083(13) C3 0.0282(13) 0.0433(16) 0.0279(13) 0.0149(12) 0.0039(11) 0.0084(12) C4 0.070(2) 0.0445(19) 0.0280(15) -0.0036(13) 0.0064(15) 0.0053(17) C5 0.0520(19) 0.0468(18) 0.0365(16) 0.0206(14) 0.0069(14) 0.0105(15) C6 0.0315(14) 0.0436(16) 0.0269(13) 0.0073(12) 0.0083(11) -0.0028(12) C7 0.0355(15) 0.0478(18) 0.0347(15) 0.0003(13) 0.0160(13) 0.0056(13) C8 0.0348(15) 0.0398(16) 0.0336(15) 0.0046(12) 0.0107(12) 0.0115(12) C9 0.059(2) 0.051(2) 0.0389(17) 0.0158(15) 0.0185(16) -0.0074(16) C10 0.082(3) 0.050(2) 0.060(2) 0.0144(18) 0.033(2) 0.035(2) C11 0.0292(13) 0.0292(13) 0.0215(12) 0.0070(10) 0.0053(10) 0.0065(10) C12 0.0272(13) 0.0322(14) 0.0219(12) 0.0084(10) 0.0062(10) 0.0034(10) C13 0.0245(12) 0.0350(14) 0.0232(12) 0.0063(10) 0.0067(10) 0.0019(10) C14 0.0283(14) 0.0438(16) 0.0268(13) 0.0061(12) 0.0072(11) 0.0040(12) C15 0.0275(14) 0.0484(17) 0.0285(14) 0.0058(13) 0.0040(11) -0.0039(12) C16 0.0358(15) 0.0389(16) 0.0273(13) 0.0103(12) 0.0064(11) -0.0029(12) C17 0.0356(14) 0.0322(14) 0.0227(12) 0.0089(11) 0.0041(11) 0.0014(11) C18 0.0283(14) 0.0527(19) 0.0340(15) 0.0002(13) 0.0042(12) 0.0119(13) C19 0.0343(16) 0.066(2) 0.0382(17) -0.0019(15) 0.0094(13) 0.0137(15) C20 0.0420(18) 0.0480(19) 0.0425(18) 0.0068(15) 0.0001(14) 0.0185(15) C21 0.0274(16) 0.071(3) 0.056(2) -0.0012(18) 0.0025(15) 0.0126(16) C22 0.0410(17) 0.0427(17) 0.0385(17) 0.0120(14) 0.0005(13) -0.0092(13) C23 0.059(2) 0.048(2) 0.0391(18) 0.0070(15) -0.0013(16) -0.0097(17) C24 0.069(3) 0.072(3) 0.061(3) 0.023(2) 0.018(2) -0.021(2) C25 0.056(2) 0.0387(19) 0.089(3) 0.012(2) -0.005(2) -0.0058(17) C26 0.054(2) 0.046(2) 0.064(2) 0.0019(18) 0.0104(19) 0.0211(17) C27 0.087(3) 0.068(3) 0.054(2) 0.025(2) 0.004(2) 0.019(2) C28 0.089(4) 0.040(2) 0.126(5) 0.032(3) 0.004(3) 0.009(2) C29 0.123(5) 0.059(3) 0.117(5) 0.003(3) 0.081(4) -0.021(3) C30 0.0312(17) 0.058(2) 0.097(3) -0.012(2) 0.0207(19) 0.0040(16) C31 0.050(2) 0.050(2) 0.076(3) -0.011(2) 0.008(2) -0.0030(17) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.4306(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn1 . O1 . 1.936(2) yes Zn1 . N1 . 2.061(2) yes Zn1 . N3 . 2.080(2) yes Zn1 . N5 . 1.923(3) yes O1 . C13 . 1.317(3) yes N1 . N2 . 1.367(3) yes N1 . C1 . 1.335(4) yes N2 . C3 . 1.357(3) yes N2 . C11 . 1.460(3) yes N3 . N4 . 1.369(3) yes N3 . C6 . 1.328(4) yes N4 . C8 . 1.358(4) yes N4 . C11 . 1.464(3) yes N5 . Si1 . 1.707(3) yes N5 . Si2 . 1.702(3) yes Si1 . C26 . 1.850(5) yes Si1 . C27 . 1.871(4) yes Si1 . C28 . 1.886(4) yes Si2 . C29 . 1.888(5) yes Si2 . C30 . 1.861(5) yes Si2 . C31 . 1.884(4) yes C1 . C2 . 1.400(4) yes C1 . C4 . 1.488(4) yes C2 . C3 . 1.376(4) yes C2 . H21 . 1.000 no C3 . C5 . 1.492(4) yes C4 . H41 . 1.000 no C4 . H42 . 1.000 no C4 . H43 . 1.000 no C5 . H51 . 1.000 no C5 . H52 . 1.000 no C5 . H53 . 1.000 no C6 . C7 . 1.401(5) yes C6 . C9 . 1.493(5) yes C7 . C8 . 1.372(5) yes C7 . H71 . 1.000 no C8 . C10 . 1.500(5) yes C9 . H91 . 1.000 no C9 . H92 . 1.000 no C9 . H93 . 1.000 no C10 . H101 . 1.000 no C10 . H102 . 1.000 no C10 . H103 . 1.000 no C11 . C12 . 1.519(4) yes C11 . H111 . 1.000 no C12 . C13 . 1.420(4) yes C12 . C17 . 1.402(4) yes C13 . C14 . 1.439(4) yes C14 . C15 . 1.390(4) yes C14 . C18 . 1.541(4) yes C15 . C16 . 1.391(5) yes C15 . H151 . 1.000 no C16 . C17 . 1.389(4) yes C16 . C22 . 1.529(4) yes C17 . H171 . 1.000 no C18 . C19 . 1.534(4) yes C18 . C20 . 1.527(5) yes C18 . C21 . 1.542(4) yes C19 . H191 . 1.000 no C19 . H192 . 1.000 no C19 . H193 . 1.000 no C20 . H201 . 1.000 no C20 . H202 . 1.000 no C20 . H203 . 1.000 no C21 . H211 . 1.000 no C21 . H212 . 1.000 no C21 . H213 . 1.000 no C22 . C23 . 1.515(5) yes C22 . C24 . 1.537(5) yes C22 . C25 . 1.522(6) yes C23 . H231 . 1.000 no C23 . H232 . 1.000 no C23 . H233 . 1.000 no C24 . H241 . 1.000 no C24 . H242 . 1.000 no C24 . H243 . 1.000 no C25 . H251 . 1.000 no C25 . H252 . 1.000 no C25 . H253 . 1.000 no C26 . H261 . 1.000 no C26 . H262 . 1.000 no C26 . H263 . 1.000 no C27 . H271 . 1.000 no C27 . H272 . 1.000 no C27 . H273 . 1.000 no C28 . H281 . 1.000 no C28 . H282 . 1.000 no C28 . H283 . 1.000 no C29 . H291 . 1.000 no C29 . H292 . 1.000 no C29 . H293 . 1.000 no C30 . H301 . 1.000 no C30 . H302 . 1.000 no C30 . H303 . 1.000 no C31 . H311 . 1.000 no C31 . H312 . 1.000 no C31 . H313 . 1.000 no C101 . C107 2_655 1.513(5) yes C101 . C106 2_655 1.409(5) yes C101 . C102 2_655 1.406(5) yes C101 . C102 . 1.406(5) yes C101 . C106 . 1.409(5) yes C101 . C107 . 1.513(5) yes C102 . C103 . 1.408(5) yes C102 . H1021 . 1.000 no C103 . C104 . 1.406(5) yes C103 . H1031 . 1.000 no C104 . C105 . 1.404(5) yes C104 . H1041 . 1.000 no C105 . C106 . 1.402(5) yes C105 . H1051 . 1.000 no C106 . H1061 . 1.000 no C107 . H1071 . 1.000 no C107 . H1072 . 1.000 no C107 . H1073 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . Zn1 . N1 . 91.27(9) yes O1 . Zn1 . N3 . 96.78(9) yes N1 . Zn1 . N3 . 91.55(9) yes O1 . Zn1 . N5 . 126.18(10) yes N1 . Zn1 . N5 . 121.61(10) yes N3 . Zn1 . N5 . 120.80(11) yes Zn1 . O1 . C13 . 131.78(17) yes Zn1 . N1 . N2 . 117.45(16) yes Zn1 . N1 . C1 . 136.3(2) yes N2 . N1 . C1 . 105.8(2) yes N1 . N2 . C3 . 111.2(2) yes N1 . N2 . C11 . 121.7(2) yes C3 . N2 . C11 . 127.0(2) yes Zn1 . N3 . N4 . 115.85(16) yes Zn1 . N3 . C6 . 136.9(2) yes N4 . N3 . C6 . 105.8(2) yes N3 . N4 . C8 . 111.1(2) yes N3 . N4 . C11 . 120.5(2) yes C8 . N4 . C11 . 127.1(2) yes Zn1 . N5 . Si1 . 114.83(15) yes Zn1 . N5 . Si2 . 119.76(15) yes Si1 . N5 . Si2 . 125.25(16) yes N5 . Si1 . C26 . 111.26(16) yes N5 . Si1 . C27 . 110.17(18) yes C26 . Si1 . C27 . 109.3(2) yes N5 . Si1 . C28 . 113.9(2) yes C26 . Si1 . C28 . 105.4(3) yes C27 . Si1 . C28 . 106.6(3) yes N5 . Si2 . C29 . 112.8(2) yes N5 . Si2 . C30 . 110.18(16) yes C29 . Si2 . C30 . 106.8(3) yes N5 . Si2 . C31 . 113.33(17) yes C29 . Si2 . C31 . 105.9(2) yes C30 . Si2 . C31 . 107.5(2) yes N1 . C1 . C2 . 110.2(3) yes N1 . C1 . C4 . 120.4(3) yes C2 . C1 . C4 . 129.4(3) yes C1 . C2 . C3 . 106.3(3) yes C1 . C2 . H21 . 127.0 no C3 . C2 . H21 . 126.7 no C2 . C3 . N2 . 106.5(3) yes C2 . C3 . C5 . 130.2(3) yes N2 . C3 . C5 . 123.2(3) yes C1 . C4 . H41 . 108.6 no C1 . C4 . H42 . 108.0 no H41 . C4 . H42 . 109.5 no C1 . C4 . H43 . 110.0 no H41 . C4 . H43 . 110.4 no H42 . C4 . H43 . 110.4 no C3 . C5 . H51 . 109.4 no C3 . C5 . H52 . 109.6 no H51 . C5 . H52 . 109.5 no C3 . C5 . H53 . 109.4 no H51 . C5 . H53 . 109.5 no H52 . C5 . H53 . 109.5 no N3 . C6 . C7 . 110.4(3) yes N3 . C6 . C9 . 121.3(3) yes C7 . C6 . C9 . 128.4(3) yes C6 . C7 . C8 . 106.3(3) yes C6 . C7 . H71 . 127.2 no C8 . C7 . H71 . 126.5 no C7 . C8 . N4 . 106.5(3) yes C7 . C8 . C10 . 130.6(3) yes N4 . C8 . C10 . 122.8(3) yes C6 . C9 . H91 . 110.0 no C6 . C9 . H92 . 109.1 no H91 . C9 . H92 . 109.5 no C6 . C9 . H93 . 109.3 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no C8 . C10 . H101 . 109.7 no C8 . C10 . H102 . 108.9 no H101 . C10 . H102 . 109.5 no C8 . C10 . H103 . 109.8 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no N4 . C11 . N2 . 110.3(2) yes N4 . C11 . C12 . 113.9(2) yes N2 . C11 . C12 . 117.0(2) yes N4 . C11 . H111 . 104.7 no N2 . C11 . H111 . 104.8 no C12 . C11 . H111 . 104.8 no C11 . C12 . C13 . 125.2(2) yes C11 . C12 . C17 . 114.1(2) yes C13 . C12 . C17 . 120.7(2) yes C12 . C13 . O1 . 123.8(2) yes C12 . C13 . C14 . 117.1(2) yes O1 . C13 . C14 . 119.1(2) yes C13 . C14 . C15 . 118.7(3) yes C13 . C14 . C18 . 120.2(3) yes C15 . C14 . C18 . 121.1(3) yes C14 . C15 . C16 . 124.8(3) yes C14 . C15 . H151 . 117.7 no C16 . C15 . H151 . 117.5 no C15 . C16 . C17 . 115.9(3) yes C15 . C16 . C22 . 119.8(3) yes C17 . C16 . C22 . 124.3(3) yes C12 . C17 . C16 . 122.7(3) yes C12 . C17 . H171 . 118.9 no C16 . C17 . H171 . 118.4 no C14 . C18 . C19 . 109.4(3) yes C14 . C18 . C20 . 110.9(3) yes C19 . C18 . C20 . 110.4(3) yes C14 . C18 . C21 . 112.3(3) yes C19 . C18 . C21 . 106.9(3) yes C20 . C18 . C21 . 106.9(3) yes C18 . C19 . H191 . 110.0 no C18 . C19 . H192 . 109.4 no H191 . C19 . H192 . 109.5 no C18 . C19 . H193 . 109.0 no H191 . C19 . H193 . 109.5 no H192 . C19 . H193 . 109.5 no C18 . C20 . H201 . 109.6 no C18 . C20 . H202 . 109.5 no H201 . C20 . H202 . 109.5 no C18 . C20 . H203 . 109.3 no H201 . C20 . H203 . 109.5 no H202 . C20 . H203 . 109.5 no C18 . C21 . H211 . 109.6 no C18 . C21 . H212 . 109.4 no H211 . C21 . H212 . 109.5 no C18 . C21 . H213 . 109.4 no H211 . C21 . H213 . 109.5 no H212 . C21 . H213 . 109.5 no C16 . C22 . C23 . 109.5(3) yes C16 . C22 . C24 . 109.9(3) yes C23 . C22 . C24 . 108.7(3) yes C16 . C22 . C25 . 111.9(3) yes C23 . C22 . C25 . 108.7(3) yes C24 . C22 . C25 . 108.1(4) yes C22 . C23 . H231 . 109.4 no C22 . C23 . H232 . 109.7 no H231 . C23 . H232 . 109.5 no C22 . C23 . H233 . 109.3 no H231 . C23 . H233 . 109.5 no H232 . C23 . H233 . 109.5 no C22 . C24 . H241 . 110.0 no C22 . C24 . H242 . 109.5 no H241 . C24 . H242 . 109.5 no C22 . C24 . H243 . 108.9 no H241 . C24 . H243 . 109.5 no H242 . C24 . H243 . 109.5 no C22 . C25 . H251 . 109.7 no C22 . C25 . H252 . 109.3 no H251 . C25 . H252 . 109.5 no C22 . C25 . H253 . 109.3 no H251 . C25 . H253 . 109.5 no H252 . C25 . H253 . 109.5 no Si1 . C26 . H261 . 109.7 no Si1 . C26 . H262 . 109.4 no H261 . C26 . H262 . 109.5 no Si1 . C26 . H263 . 109.3 no H261 . C26 . H263 . 109.5 no H262 . C26 . H263 . 109.5 no Si1 . C27 . H271 . 109.7 no Si1 . C27 . H272 . 109.8 no H271 . C27 . H272 . 109.5 no Si1 . C27 . H273 . 108.9 no H271 . C27 . H273 . 109.5 no H272 . C27 . H273 . 109.5 no Si1 . C28 . H281 . 110.0 no Si1 . C28 . H282 . 109.4 no H281 . C28 . H282 . 109.5 no Si1 . C28 . H283 . 109.0 no H281 . C28 . H283 . 109.5 no H282 . C28 . H283 . 109.5 no Si2 . C29 . H291 . 109.6 no Si2 . C29 . H292 . 109.4 no H291 . C29 . H292 . 109.5 no Si2 . C29 . H293 . 109.4 no H291 . C29 . H293 . 109.5 no H292 . C29 . H293 . 109.5 no Si2 . C30 . H301 . 109.3 no Si2 . C30 . H302 . 109.4 no H301 . C30 . H302 . 109.5 no Si2 . C30 . H303 . 109.7 no H301 . C30 . H303 . 109.5 no H302 . C30 . H303 . 109.5 no Si2 . C31 . H311 . 109.4 no Si2 . C31 . H312 . 109.6 no H311 . C31 . H312 . 109.5 no Si2 . C31 . H313 . 109.4 no H311 . C31 . H313 . 109.5 no H312 . C31 . H313 . 109.5 no C107 2_655 C101 . C106 2_655 120.00(19) yes C107 2_655 C101 . C102 2_655 119.83(19) yes C106 2_655 C101 . C102 2_655 119.9(3) yes C107 2_655 C101 . C102 . 60.17(19) yes C106 2_655 C101 . C102 . 60.1(3) yes C102 2_655 C101 . C102 . 179.992 yes C107 2_655 C101 . C106 . 60.00(19) yes C106 2_655 C101 . C106 . 179.992 yes C102 2_655 C101 . C106 . 60.1(3) yes C102 . C101 . C106 . 119.9(3) yes C107 2_655 C101 . C107 . 179.992 yes C106 2_655 C101 . C107 . 60.00(19) yes C102 2_655 C101 . C107 . 60.17(19) yes C102 . C101 . C107 . 119.83(19) yes C106 . C101 . C107 . 120.00(19) yes C101 . C102 . C103 . 120.6(6) yes C101 . C102 . H1021 . 121.3 no C103 . C102 . H1021 . 118.1 no C102 . C103 . C104 . 119.2(7) yes C102 . C103 . H1031 . 121.7 no C104 . C103 . H1031 . 119.1 no C103 . C104 . C105 . 120.0(7) yes C103 . C104 . H1041 . 121.6 no C105 . C104 . H1041 . 118.3 no C104 . C105 . C106 . 120.8(7) yes C104 . C105 . H1051 . 121.2 no C106 . C105 . H1051 . 117.8 no C101 . C106 . C105 . 119.2(6) yes C101 . C106 . H1061 . 119.1 no C105 . C106 . H1061 . 121.7 no C101 . C107 . H1071 . 110.9 no C101 . C107 . H1072 . 108.3 no H1071 . C107 . H1072 . 109.5 no C101 . C107 . H1073 . 109.2 no H1071 . C107 . H1073 . 109.5 no H1072 . C107 . H1073 . 109.5 no _chemical_name_common Zn((Me2pz)2C(C6H2(tBu)2O)(N(SiMe3)2).0.35(C7H8) #===end data_compound_11 _database_code_depnum_ccdc_archive 'CCDC 696843' # Local code mgc15 _chemical_name_systematic ; Zn((pz)2CArO)Cl ; _publ_section_exptl_refinement ; no special details ; _chemical_melting_point ? _cell_length_a 9.81900(10) _cell_length_b 23.2485(3) _cell_length_c 11.11250(10) _cell_angle_alpha 90 _cell_angle_beta 94.5044(6) _cell_angle_gamma 90 _cell_volume 2528.89(5) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Zn 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C25 H35 Cl1 N4 O1 Zn1' _chemical_formula_moiety 'C25 H35 Cl1 N4 O1 Zn1' _chemical_compound_source ? _chemical_formula_weight 508.41 _cell_measurement_reflns_used 5889 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_meas ? _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 1.101 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 0.90 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 11508 _reflns_number_total 5771 _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_theta_min 5.133 _diffrn_reflns_theta_max 27.511 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.961 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 30 _reflns_limit_l_min 0 _reflns_limit_l_max 14 _oxford_diffrn_Wilson_B_factor 2.02 _oxford_diffrn_Wilson_scale 12.23 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.41 _refine_diff_density_max 0.30 _refine_ls_number_reflns 4156 _refine_ls_number_restraints 0 _refine_ls_number_parameters 289 _refine_ls_wR_factor_ref 0.0317 _refine_ls_goodness_of_fit_ref 1.1216 _refine_ls_R_factor_all 0.0496 _refine_ls_wR_factor_all 0.0387 _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 4156 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_gt 0.0317 _refine_ls_shift/su_max 0.000996 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.08 1.22 1.16 0.463 0.298 ; 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Zn1 Zn 0.84342(2) 0.561552(10) 0.27527(2) 0.0227 1.0000 Uani . . . . . . Cl1 Cl 1.06009(5) 0.54824(3) 0.25403(5) 0.0390 1.0000 Uani . . . . . . O1 O 0.77723(13) 0.61162(6) 0.39391(12) 0.0256 1.0000 Uani . . . . . . N1 N 0.71658(16) 0.49526(7) 0.31438(14) 0.0230 1.0000 Uani . . . . . . N2 N 0.58102(16) 0.50995(7) 0.30616(14) 0.0210 1.0000 Uani . . . . . . N3 N 0.72258(17) 0.57717(7) 0.11975(15) 0.0242 1.0000 Uani . . . . . . N4 N 0.58537(16) 0.56898(7) 0.12835(14) 0.0217 1.0000 Uani . . . . . . C1 C 0.7245(2) 0.44438(8) 0.37053(17) 0.0242 1.0000 Uani . . . . . . C2 C 0.5944(2) 0.42641(8) 0.39767(18) 0.0260 1.0000 Uani . . . . . . C3 C 0.5046(2) 0.46912(8) 0.35687(17) 0.0228 1.0000 Uani . . . . . . C4 C 0.8612(2) 0.41691(9) 0.4010(2) 0.0338 1.0000 Uani . . . . . . C5 C 0.3547(2) 0.47523(9) 0.36438(19) 0.0272 1.0000 Uani . . . . . . C6 C 0.7384(2) 0.58759(9) 0.00372(19) 0.0285 1.0000 Uani . . . . . . C7 C 0.6097(2) 0.58775(9) -0.06165(18) 0.0295 1.0000 Uani . . . . . . C8 C 0.5145(2) 0.57584(8) 0.01906(18) 0.0256 1.0000 Uani . . . . . . C9 C 0.8766(3) 0.59633(11) -0.0405(2) 0.0386 1.0000 Uani . . . . . . C10 C 0.3626(2) 0.57046(9) -0.0002(2) 0.0312 1.0000 Uani . . . . . . C11 C 0.53068(18) 0.56328(8) 0.24689(16) 0.0205 1.0000 Uani . . . . . . C12 C 0.53972(19) 0.61855(8) 0.32045(17) 0.0197 1.0000 Uani . . . . . . C13 C 0.65766(18) 0.63825(8) 0.38998(16) 0.0194 1.0000 Uani . . . . . . C14 C 0.64377(18) 0.68943(8) 0.46030(16) 0.0199 1.0000 Uani . . . . . . C15 C 0.52264(19) 0.72022(8) 0.44497(17) 0.0202 1.0000 Uani . . . . . . C16 C 0.40893(18) 0.70340(8) 0.36884(16) 0.0194 1.0000 Uani . . . . . . C17 C 0.41898(18) 0.65112(8) 0.31097(17) 0.0201 1.0000 Uani . . . . . . C18 C 0.76205(19) 0.71162(8) 0.54743(17) 0.0217 1.0000 Uani . . . . . . C19 C 0.8830(2) 0.72835(11) 0.4759(2) 0.0351 1.0000 Uani . . . . . . C20 C 0.7216(2) 0.76488(9) 0.6186(2) 0.0297 1.0000 Uani . . . . . . C21 C 0.8071(2) 0.66535(9) 0.64057(19) 0.0300 1.0000 Uani . . . . . . C22 C 0.28658(19) 0.74424(8) 0.34757(17) 0.0216 1.0000 Uani . . . . . . C23 C 0.2396(2) 0.76541(9) 0.46766(19) 0.0287 1.0000 Uani . . . . . . C24 C 0.3337(2) 0.79648(9) 0.2769(2) 0.0295 1.0000 Uani . . . . . . C25 C 0.16484(19) 0.71514(9) 0.27734(18) 0.0251 1.0000 Uani . . . . . . H21 H 0.5709 0.3898 0.4384 0.0309 1.0000 Uiso R . . . . . H41 H 0.8487 0.3794 0.4426 0.0400 1.0000 Uiso R . . . . . H42 H 0.9187 0.4430 0.4555 0.0400 1.0000 Uiso R . . . . . H43 H 0.9073 0.4102 0.3252 0.0400 1.0000 Uiso R . . . . . H51 H 0.3188 0.4406 0.4049 0.0333 1.0000 Uiso R . . . . . H52 H 0.3355 0.5104 0.4119 0.0333 1.0000 Uiso R . . . . . H53 H 0.3089 0.4787 0.2811 0.0333 1.0000 Uiso R . . . . . H71 H 0.5910 0.5951 -0.1501 0.0352 1.0000 Uiso R . . . . . H101 H 0.3330 0.5771 -0.0873 0.0377 1.0000 Uiso R . . . . . H102 H 0.3189 0.5998 0.0502 0.0377 1.0000 Uiso R . . . . . H103 H 0.3343 0.5311 0.0238 0.0377 1.0000 Uiso R . . . . . H111 H 0.4306 0.5567 0.2283 0.0248 1.0000 Uiso R . . . . . H151 H 0.5159 0.7568 0.4916 0.0246 1.0000 Uiso R . . . . . H171 H 0.3377 0.6360 0.2610 0.0245 1.0000 Uiso R . . . . . H191 H 0.9595 0.7428 0.5327 0.0443 1.0000 Uiso R . . . . . H192 H 0.8542 0.7593 0.4167 0.0443 1.0000 Uiso R . . . . . H193 H 0.9144 0.6940 0.4316 0.0443 1.0000 Uiso R . . . . . H201 H 0.8012 0.7777 0.6738 0.0370 1.0000 Uiso R . . . . . H202 H 0.6936 0.7966 0.5612 0.0370 1.0000 Uiso R . . . . . H203 H 0.6435 0.7549 0.6674 0.0370 1.0000 Uiso R . . . . . H211 H 0.8837 0.6806 0.6961 0.0366 1.0000 Uiso R . . . . . H212 H 0.7286 0.6548 0.6883 0.0366 1.0000 Uiso R . . . . . H213 H 0.8388 0.6305 0.5981 0.0366 1.0000 Uiso R . . . . . H231 H 0.1600 0.7919 0.4523 0.0360 1.0000 Uiso R . . . . . H232 H 0.3162 0.7863 0.5134 0.0360 1.0000 Uiso R . . . . . H233 H 0.2119 0.7317 0.5160 0.0360 1.0000 Uiso R . . . . . H241 H 0.2558 0.8239 0.2617 0.0356 1.0000 Uiso R . . . . . H242 H 0.4104 0.8161 0.3252 0.0356 1.0000 Uiso R . . . . . H243 H 0.3657 0.7834 0.1981 0.0356 1.0000 Uiso R . . . . . H251 H 0.0875 0.7431 0.2653 0.0316 1.0000 Uiso R . . . . . H252 H 0.1923 0.7021 0.1970 0.0316 1.0000 Uiso R . . . . . H253 H 0.1352 0.6812 0.3241 0.0316 1.0000 Uiso R . . . . . H91 H 0.9464 0.5976 0.0301 0.0476 1.0000 Uiso R . . . . . H92 H 0.8976 0.5637 -0.0945 0.0476 1.0000 Uiso R . . . . . H93 H 0.8784 0.6333 -0.0863 0.0476 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02009(11) 0.02453(12) 0.02336(12) -0.00287(9) 0.00062(8) 0.00312(9) Cl1 0.0221(2) 0.0497(3) 0.0456(3) -0.0065(3) 0.0042(2) 0.0068(2) O1 0.0206(7) 0.0295(7) 0.0258(7) -0.0057(6) -0.0032(5) 0.0062(5) N1 0.0236(8) 0.0231(8) 0.0217(8) -0.0009(6) -0.0010(6) 0.0045(6) N2 0.0225(8) 0.0187(8) 0.0214(8) -0.0001(6) -0.0004(6) 0.0025(6) N3 0.0273(8) 0.0236(8) 0.0216(8) -0.0004(6) 0.0012(6) 0.0021(6) N4 0.0248(8) 0.0221(8) 0.0177(7) -0.0012(6) -0.0020(6) 0.0025(6) C1 0.0332(10) 0.0195(9) 0.0191(9) -0.0035(7) -0.0021(7) 0.0050(8) C2 0.0356(11) 0.0209(10) 0.0210(9) -0.0012(7) -0.0011(8) 0.0005(8) C3 0.0295(10) 0.0199(9) 0.0186(9) -0.0038(7) -0.0008(7) -0.0012(7) C4 0.0360(12) 0.0266(10) 0.0370(12) 0.0000(9) -0.0082(9) 0.0082(9) C5 0.0279(10) 0.0268(10) 0.0270(10) -0.0036(8) 0.0029(8) -0.0032(8) C6 0.0401(12) 0.0203(9) 0.0254(10) 0.0001(8) 0.0047(8) 0.0033(8) C7 0.0444(12) 0.0237(10) 0.0199(10) -0.0002(8) -0.0008(8) 0.0050(9) C8 0.0365(11) 0.0170(9) 0.0221(10) -0.0029(7) -0.0055(8) 0.0052(7) C9 0.0459(14) 0.0399(13) 0.0312(12) 0.0038(10) 0.0111(10) 0.0027(10) C10 0.0354(11) 0.0261(11) 0.0298(11) -0.0030(8) -0.0113(9) 0.0040(8) C11 0.0202(9) 0.0198(8) 0.0210(9) -0.0005(7) -0.0021(7) 0.0035(7) C12 0.0229(9) 0.0174(9) 0.0184(9) -0.0007(7) 0.0004(7) 0.0001(7) C13 0.0194(9) 0.0208(9) 0.0180(9) 0.0014(7) 0.0020(7) 0.0023(7) C14 0.0192(8) 0.0212(9) 0.0192(9) 0.0001(7) 0.0013(7) -0.0020(7) C15 0.0231(9) 0.0192(9) 0.0186(9) -0.0005(7) 0.0029(7) -0.0003(7) C16 0.0191(8) 0.0206(9) 0.0187(9) 0.0028(7) 0.0034(7) 0.0021(7) C17 0.0189(9) 0.0226(9) 0.0186(9) 0.0004(7) -0.0004(7) 0.0007(7) C18 0.0209(9) 0.0232(9) 0.0208(9) -0.0031(7) -0.0005(7) -0.0018(7) C19 0.0259(11) 0.0456(13) 0.0342(12) -0.0049(10) 0.0053(9) -0.0126(9) C20 0.0302(11) 0.0268(10) 0.0309(11) -0.0080(8) -0.0041(8) -0.0010(8) C21 0.0345(11) 0.0293(11) 0.0244(10) -0.0004(8) -0.0094(8) 0.0006(9) C22 0.0207(9) 0.0223(9) 0.0218(9) 0.0001(7) 0.0012(7) 0.0033(7) C23 0.0258(10) 0.0316(11) 0.0288(11) -0.0044(8) 0.0023(8) 0.0065(8) C24 0.0310(10) 0.0247(9) 0.0325(11) 0.0048(9) 0.0003(8) 0.0011(9) C25 0.0203(9) 0.0293(10) 0.0253(10) 0.0012(8) -0.0006(7) 0.0029(8) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2803(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn1 . Cl1 . 2.1810(5) yes Zn1 . O1 . 1.9105(14) yes Zn1 . N1 . 2.0494(17) yes Zn1 . N3 . 2.0505(16) yes O1 . C13 . 1.325(2) yes N1 . N2 . 1.370(2) yes N1 . C1 . 1.337(3) yes N2 . C3 . 1.359(2) yes N2 . C11 . 1.471(2) yes N3 . N4 . 1.371(2) yes N3 . C6 . 1.333(3) yes N4 . C8 . 1.361(2) yes N4 . C11 . 1.467(2) yes C1 . C2 . 1.400(3) yes C1 . C4 . 1.501(3) yes C2 . C3 . 1.380(3) yes C2 . H21 . 1.000 no C3 . C5 . 1.488(3) yes C4 . H41 . 1.000 no C4 . H42 . 1.000 no C4 . H43 . 1.000 no C5 . H51 . 1.000 no C5 . H52 . 1.000 no C5 . H53 . 1.000 no C6 . C7 . 1.407(3) yes C6 . C9 . 1.493(3) yes C7 . C8 . 1.373(3) yes C7 . H71 . 1.000 no C8 . C10 . 1.496(3) yes C9 . H91 . 1.000 no C9 . H92 . 1.000 no C9 . H93 . 1.000 no C10 . H101 . 1.000 no C10 . H102 . 1.000 no C10 . H103 . 1.000 no C11 . C12 . 1.522(2) yes C11 . H111 . 1.000 no C12 . C13 . 1.417(3) yes C12 . C17 . 1.404(3) yes C13 . C14 . 1.436(3) yes C14 . C15 . 1.387(3) yes C14 . C18 . 1.541(2) yes C15 . C16 . 1.402(3) yes C15 . H151 . 1.000 no C16 . C17 . 1.382(3) yes C16 . C22 . 1.535(2) yes C17 . H171 . 1.000 no C18 . C19 . 1.531(3) yes C18 . C20 . 1.539(3) yes C18 . C21 . 1.534(3) yes C19 . H191 . 1.000 no C19 . H192 . 1.000 no C19 . H193 . 1.000 no C20 . H201 . 1.000 no C20 . H202 . 1.000 no C20 . H203 . 1.000 no C21 . H211 . 1.000 no C21 . H212 . 1.000 no C21 . H213 . 1.000 no C22 . C23 . 1.527(3) yes C22 . C24 . 1.537(3) yes C22 . C25 . 1.533(3) yes C23 . H231 . 1.000 no C23 . H232 . 1.000 no C23 . H233 . 1.000 no C24 . H241 . 1.000 no C24 . H242 . 1.000 no C24 . H243 . 1.000 no C25 . H251 . 1.000 no C25 . H252 . 1.000 no C25 . H253 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Zn1 . O1 . 123.28(4) yes Cl1 . Zn1 . N1 . 122.04(5) yes O1 . Zn1 . N1 . 93.81(6) yes Cl1 . Zn1 . N3 . 116.02(5) yes O1 . Zn1 . N3 . 105.55(6) yes N1 . Zn1 . N3 . 89.48(6) yes Zn1 . O1 . C13 . 127.63(12) yes Zn1 . N1 . N2 . 113.70(12) yes Zn1 . N1 . C1 . 138.61(13) yes N2 . N1 . C1 . 105.80(16) yes N1 . N2 . C3 . 111.29(15) yes N1 . N2 . C11 . 122.02(15) yes C3 . N2 . C11 . 126.67(16) yes Zn1 . N3 . N4 . 115.04(12) yes Zn1 . N3 . C6 . 138.07(14) yes N4 . N3 . C6 . 106.39(16) yes N3 . N4 . C8 . 110.96(16) yes N3 . N4 . C11 . 120.39(15) yes C8 . N4 . C11 . 127.92(16) yes N1 . C1 . C2 . 110.11(17) yes N1 . C1 . C4 . 120.02(18) yes C2 . C1 . C4 . 129.77(18) yes C1 . C2 . C3 . 106.54(17) yes C1 . C2 . H21 . 126.8 no C3 . C2 . H21 . 126.7 no C2 . C3 . N2 . 106.24(17) yes C2 . C3 . C5 . 131.24(19) yes N2 . C3 . C5 . 122.49(17) yes C1 . C4 . H41 . 109.6 no C1 . C4 . H42 . 109.4 no H41 . C4 . H42 . 109.5 no C1 . C4 . H43 . 109.4 no H41 . C4 . H43 . 109.5 no H42 . C4 . H43 . 109.5 no C3 . C5 . H51 . 109.5 no C3 . C5 . H52 . 109.6 no H51 . C5 . H52 . 109.5 no C3 . C5 . H53 . 109.3 no H51 . C5 . H53 . 109.5 no H52 . C5 . H53 . 109.5 no N3 . C6 . C7 . 109.39(19) yes N3 . C6 . C9 . 121.37(19) yes C7 . C6 . C9 . 129.2(2) yes C6 . C7 . C8 . 106.96(18) yes C6 . C7 . H71 . 126.5 no C8 . C7 . H71 . 126.5 no C7 . C8 . N4 . 106.27(18) yes C7 . C8 . C10 . 130.19(19) yes N4 . C8 . C10 . 123.54(19) yes C6 . C9 . H91 . 109.3 no C6 . C9 . H92 . 109.3 no H91 . C9 . H92 . 109.5 no C6 . C9 . H93 . 109.7 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no C8 . C10 . H101 . 109.7 no C8 . C10 . H102 . 109.2 no H101 . C10 . H102 . 109.5 no C8 . C10 . H103 . 109.5 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no N2 . C11 . N4 . 110.14(14) yes N2 . C11 . C12 . 117.88(15) yes N4 . C11 . C12 . 113.33(15) yes N2 . C11 . H111 . 104.7 no N4 . C11 . H111 . 104.6 no C12 . C11 . H111 . 104.8 no C11 . C12 . C13 . 125.22(16) yes C11 . C12 . C17 . 113.70(16) yes C13 . C12 . C17 . 121.05(16) yes C12 . C13 . O1 . 123.43(16) yes C12 . C13 . C14 . 117.14(16) yes O1 . C13 . C14 . 119.42(16) yes C13 . C14 . C15 . 118.55(16) yes C13 . C14 . C18 . 121.34(16) yes C15 . C14 . C18 . 120.06(16) yes C14 . C15 . C16 . 124.37(17) yes C14 . C15 . H151 . 117.7 no C16 . C15 . H151 . 117.9 no C15 . C16 . C17 . 116.31(16) yes C15 . C16 . C22 . 119.80(16) yes C17 . C16 . C22 . 123.77(16) yes C12 . C17 . C16 . 122.02(17) yes C12 . C17 . H171 . 119.0 no C16 . C17 . H171 . 119.0 no C14 . C18 . C19 . 109.64(16) yes C14 . C18 . C20 . 112.34(15) yes C19 . C18 . C20 . 107.76(17) yes C14 . C18 . C21 . 110.64(15) yes C19 . C18 . C21 . 109.52(17) yes C20 . C18 . C21 . 106.86(16) yes C18 . C19 . H191 . 109.4 no C18 . C19 . H192 . 109.5 no H191 . C19 . H192 . 109.5 no C18 . C19 . H193 . 109.5 no H191 . C19 . H193 . 109.5 no H192 . C19 . H193 . 109.5 no C18 . C20 . H201 . 109.5 no C18 . C20 . H202 . 109.5 no H201 . C20 . H202 . 109.5 no C18 . C20 . H203 . 109.4 no H201 . C20 . H203 . 109.5 no H202 . C20 . H203 . 109.5 no C18 . C21 . H211 . 109.3 no C18 . C21 . H212 . 109.6 no H211 . C21 . H212 . 109.5 no C18 . C21 . H213 . 109.5 no H211 . C21 . H213 . 109.5 no H212 . C21 . H213 . 109.5 no C16 . C22 . C23 . 110.55(16) yes C16 . C22 . C24 . 107.69(15) yes C23 . C22 . C24 . 108.38(17) yes C16 . C22 . C25 . 112.03(15) yes C23 . C22 . C25 . 108.07(16) yes C24 . C22 . C25 . 110.06(16) yes C22 . C23 . H231 . 109.6 no C22 . C23 . H232 . 109.5 no H231 . C23 . H232 . 109.5 no C22 . C23 . H233 . 109.3 no H231 . C23 . H233 . 109.5 no H232 . C23 . H233 . 109.5 no C22 . C24 . H241 . 109.5 no C22 . C24 . H242 . 109.4 no H241 . C24 . H242 . 109.5 no C22 . C24 . H243 . 109.6 no H241 . C24 . H243 . 109.5 no H242 . C24 . H243 . 109.5 no C22 . C25 . H251 . 109.5 no C22 . C25 . H252 . 109.5 no H251 . C25 . H252 . 109.5 no C22 . C25 . H253 . 109.3 no H251 . C25 . H253 . 109.5 no H252 . C25 . H253 . 109.5 no #===end _chemical_name_common Zn((pz)2CArO)Cl