# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Jean-Michel Grevy' "Miguel-\'Angel Munoz Hernandez" 'Cintya Valerio-Cardenas' _publ_contact_author_name 'Jean-Michel Grevy' _publ_contact_author_address ; Centro de Investigaciones Qu micas Universidad Aut\'onoma del estado de Morelos Avenida Universidad # 1001 Colonia Chamilpa Cuernavaca Morelos 62209 MEXICO ; _publ_contact_author_email JEANMICHELG@GMAIL.COM data_complex_2 _database_code_depnum_ccdc_archive 'CCDC 775390' #TrackingRef 'cif_complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H44 Cl4 N2 P2 Si2 Zn2' _chemical_formula_weight 847.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6601(11) _cell_length_b 11.2147(13) _cell_length_c 11.4194(14) _cell_angle_alpha 74.417(3) _cell_angle_beta 74.331(2) _cell_angle_gamma 69.169(2) _cell_volume 979.5(2) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 436 _exptl_absorpt_coefficient_mu 1.665 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6096 _exptl_absorpt_correction_T_max 0.9067 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4786 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 24.97 _reflns_number_total 3194 _reflns_number_gt 2849 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+0.9023P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3194 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1076 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.49809(6) 0.64905(4) 0.50239(4) 0.01235(16) Uani 1 1 d . . . P1 P 0.68311(12) 0.66248(10) 0.68670(9) 0.0112(2) Uani 1 1 d . . . Si1 Si 0.29794(14) 0.78185(11) 0.73217(10) 0.0138(3) Uani 1 1 d . . . N1 N 0.4993(4) 0.7023(3) 0.6563(3) 0.0108(7) Uani 1 1 d . . . Cl1 Cl 0.28928(12) 0.55064(10) 0.53386(9) 0.0156(2) Uani 1 1 d . . . Cl2 Cl 0.52551(13) 0.79590(10) 0.33164(9) 0.0196(3) Uani 1 1 d . . . C1 C 0.6972(5) 0.7403(4) 0.8010(4) 0.0129(9) Uani 1 1 d . . . C2 C 0.6957(5) 0.6750(4) 0.9243(4) 0.0157(9) Uani 1 1 d . . . H2A H 0.6903 0.5884 0.9473 0.019 Uiso 1 1 calc R . . C3 C 0.7019(5) 0.7359(4) 1.0130(4) 0.0188(10) Uani 1 1 d . . . H3A H 0.7015 0.6909 1.0964 0.023 Uiso 1 1 calc R . . C4 C 0.7087(5) 0.8627(4) 0.9797(4) 0.0224(10) Uani 1 1 d . . . H4A H 0.7118 0.9048 1.0406 0.027 Uiso 1 1 calc R . . C5 C 0.7110(5) 0.9278(4) 0.8584(4) 0.0221(10) Uani 1 1 d . . . H5A H 0.7166 1.0144 0.8360 0.027 Uiso 1 1 calc R . . C6 C 0.7052(5) 0.8674(4) 0.7684(4) 0.0189(9) Uani 1 1 d . . . H6A H 0.7066 0.9127 0.6850 0.023 Uiso 1 1 calc R . . C7 C 0.7643(5) 0.4909(4) 0.7444(3) 0.0120(9) Uani 1 1 d . . . C8 C 0.6544(5) 0.4155(4) 0.7910(4) 0.0162(9) Uani 1 1 d . . . H8A H 0.5373 0.4552 0.7918 0.019 Uiso 1 1 calc R . . C9 C 0.7151(5) 0.2838(4) 0.8359(4) 0.0183(9) Uani 1 1 d . . . H9A H 0.6396 0.2335 0.8675 0.022 Uiso 1 1 calc R . . C10 C 0.8860(5) 0.2246(4) 0.8353(4) 0.0192(10) Uani 1 1 d . . . H10A H 0.9273 0.1340 0.8664 0.023 Uiso 1 1 calc R . . C11 C 0.9968(5) 0.2983(4) 0.7890(4) 0.0202(10) Uani 1 1 d . . . H11A H 1.1139 0.2578 0.7876 0.024 Uiso 1 1 calc R . . C12 C 0.9360(5) 0.4311(4) 0.7449(4) 0.0151(9) Uani 1 1 d . . . H12A H 1.0116 0.4815 0.7149 0.018 Uiso 1 1 calc R . . C13 C 0.2946(5) 0.9003(4) 0.8210(4) 0.0207(10) Uani 1 1 d . . . H13A H 0.3593 0.8543 0.8869 0.031 Uiso 1 1 calc R . . H13B H 0.1780 0.9430 0.8577 0.031 Uiso 1 1 calc R . . H13C H 0.3447 0.9658 0.7651 0.031 Uiso 1 1 calc R . . C14 C 0.1977(6) 0.6619(4) 0.8412(4) 0.0236(10) Uani 1 1 d . . . H14A H 0.2654 0.6127 0.9048 0.035 Uiso 1 1 calc R . . H14B H 0.1908 0.6020 0.7955 0.035 Uiso 1 1 calc R . . H14C H 0.0842 0.7077 0.8807 0.035 Uiso 1 1 calc R . . C15 C 0.1718(5) 0.8772(4) 0.6095(4) 0.0223(10) Uani 1 1 d . . . H15A H 0.2260 0.9402 0.5532 0.033 Uiso 1 1 calc R . . H15B H 0.0580 0.9235 0.6482 0.033 Uiso 1 1 calc R . . H15C H 0.1654 0.8181 0.5628 0.033 Uiso 1 1 calc R . . C16 C 0.8298(5) 0.7023(4) 0.5492(4) 0.0156(9) Uani 1 1 d . . . H16A H 0.7902 0.7955 0.5149 0.023 Uiso 1 1 calc R . . H16B H 0.8389 0.6524 0.4879 0.023 Uiso 1 1 calc R . . H16C H 0.9405 0.6809 0.5700 0.023 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0115(3) 0.0123(3) 0.0119(2) -0.0022(2) -0.00156(18) -0.0026(2) P1 0.0102(5) 0.0104(6) 0.0111(5) -0.0015(4) -0.0016(4) -0.0018(4) Si1 0.0108(6) 0.0120(6) 0.0145(6) -0.0031(5) 0.0004(4) -0.0003(5) N1 0.0084(17) 0.0115(18) 0.0119(16) -0.0035(14) -0.0003(13) -0.0026(14) Cl1 0.0093(5) 0.0156(6) 0.0216(5) -0.0076(4) -0.0001(4) -0.0023(4) Cl2 0.0220(6) 0.0182(6) 0.0160(5) 0.0015(4) -0.0035(4) -0.0066(5) C1 0.0066(19) 0.015(2) 0.017(2) -0.0049(18) -0.0026(16) -0.0022(17) C2 0.012(2) 0.015(2) 0.018(2) -0.0017(18) -0.0003(17) -0.0050(18) C3 0.018(2) 0.022(3) 0.015(2) -0.0039(19) -0.0015(17) -0.0049(19) C4 0.017(2) 0.028(3) 0.025(2) -0.016(2) -0.0056(19) -0.001(2) C5 0.022(2) 0.014(2) 0.033(3) -0.009(2) -0.008(2) -0.0018(19) C6 0.017(2) 0.018(2) 0.022(2) -0.005(2) -0.0076(18) -0.0024(19) C7 0.015(2) 0.013(2) 0.0063(18) -0.0032(17) -0.0031(16) -0.0002(17) C8 0.013(2) 0.015(2) 0.020(2) -0.0059(19) -0.0029(17) -0.0008(18) C9 0.020(2) 0.013(2) 0.020(2) -0.0010(19) -0.0028(18) -0.0052(19) C10 0.023(2) 0.009(2) 0.021(2) -0.0027(19) -0.0082(19) 0.0033(18) C11 0.012(2) 0.021(3) 0.022(2) -0.003(2) -0.0068(18) 0.0041(19) C12 0.015(2) 0.013(2) 0.014(2) -0.0008(18) -0.0009(17) -0.0034(18) C13 0.015(2) 0.021(3) 0.023(2) -0.011(2) -0.0013(18) 0.0010(19) C14 0.018(2) 0.018(3) 0.026(2) -0.008(2) 0.0075(19) -0.0015(19) C15 0.015(2) 0.020(3) 0.026(2) -0.009(2) -0.0025(19) 0.0038(19) C16 0.011(2) 0.018(2) 0.016(2) -0.0034(18) 0.0007(16) -0.0055(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 2.005(3) . ? Zn1 Cl2 2.2076(11) . ? Zn1 Cl1 2.3393(10) . ? Zn1 Cl1 2.3939(11) 2_666 ? P1 N1 1.601(3) . ? P1 C16 1.797(4) . ? P1 C7 1.800(4) . ? P1 C1 1.804(4) . ? Si1 N1 1.755(3) . ? Si1 C14 1.860(4) . ? Si1 C13 1.864(4) . ? Si1 C15 1.868(5) . ? Cl1 Zn1 2.3939(11) 2_666 ? C1 C6 1.395(6) . ? C1 C2 1.400(6) . ? C2 C3 1.387(5) . ? C2 H2A 0.9500 . ? C3 C4 1.389(6) . ? C3 H3A 0.9500 . ? C4 C5 1.380(6) . ? C4 H4A 0.9500 . ? C5 C6 1.394(6) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C12 1.398(6) . ? C7 C8 1.401(5) . ? C8 C9 1.381(6) . ? C8 H8A 0.9500 . ? C9 C10 1.389(6) . ? C9 H9A 0.9500 . ? C10 C11 1.392(6) . ? C10 H10A 0.9500 . ? C11 C12 1.390(6) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn1 Cl2 114.16(10) . . ? N1 Zn1 Cl1 111.96(9) . . ? Cl2 Zn1 Cl1 117.54(4) . . ? N1 Zn1 Cl1 113.49(10) . 2_666 ? Cl2 Zn1 Cl1 107.18(4) . 2_666 ? Cl1 Zn1 Cl1 90.02(4) . 2_666 ? N1 P1 C16 110.42(18) . . ? N1 P1 C7 112.37(18) . . ? C16 P1 C7 106.89(19) . . ? N1 P1 C1 115.22(17) . . ? C16 P1 C1 106.21(18) . . ? C7 P1 C1 105.19(18) . . ? N1 Si1 C14 110.55(18) . . ? N1 Si1 C13 114.38(17) . . ? C14 Si1 C13 107.9(2) . . ? N1 Si1 C15 106.88(17) . . ? C14 Si1 C15 110.5(2) . . ? C13 Si1 C15 106.5(2) . . ? P1 N1 Si1 132.60(19) . . ? P1 N1 Zn1 113.85(16) . . ? Si1 N1 Zn1 113.55(17) . . ? Zn1 Cl1 Zn1 89.98(4) . 2_666 ? C6 C1 C2 119.3(4) . . ? C6 C1 P1 120.4(3) . . ? C2 C1 P1 120.3(3) . . ? C3 C2 C1 120.4(4) . . ? C3 C2 H2A 119.8 . . ? C1 C2 H2A 119.8 . . ? C2 C3 C4 119.8(4) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? C5 C4 C3 120.2(4) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? C4 C5 C6 120.4(4) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C5 C6 C1 119.9(4) . . ? C5 C6 H6A 120.1 . . ? C1 C6 H6A 120.1 . . ? C12 C7 C8 119.1(4) . . ? C12 C7 P1 121.1(3) . . ? C8 C7 P1 119.9(3) . . ? C9 C8 C7 120.4(4) . . ? C9 C8 H8A 119.8 . . ? C7 C8 H8A 119.8 . . ? C8 C9 C10 120.4(4) . . ? C8 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? C9 C10 C11 119.8(4) . . ? C9 C10 H10A 120.1 . . ? C11 C10 H10A 120.1 . . ? C12 C11 C10 120.0(4) . . ? C12 C11 H11A 120.0 . . ? C10 C11 H11A 120.0 . . ? C11 C12 C7 120.3(4) . . ? C11 C12 H12A 119.8 . . ? C7 C12 H12A 119.8 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? P1 C16 H16A 109.5 . . ? P1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? P1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 P1 N1 Si1 -135.2(3) . . . . ? C7 P1 N1 Si1 105.6(3) . . . . ? C1 P1 N1 Si1 -14.9(3) . . . . ? C16 P1 N1 Zn1 45.7(2) . . . . ? C7 P1 N1 Zn1 -73.5(2) . . . . ? C1 P1 N1 Zn1 166.00(18) . . . . ? C14 Si1 N1 P1 -92.4(3) . . . . ? C13 Si1 N1 P1 29.6(4) . . . . ? C15 Si1 N1 P1 147.3(3) . . . . ? C14 Si1 N1 Zn1 86.8(2) . . . . ? C13 Si1 N1 Zn1 -151.23(19) . . . . ? C15 Si1 N1 Zn1 -33.6(2) . . . . ? Cl2 Zn1 N1 P1 -89.67(18) . . . . ? Cl1 Zn1 N1 P1 133.67(15) . . . . ? Cl1 Zn1 N1 P1 33.5(2) 2_666 . . . ? Cl2 Zn1 N1 Si1 91.01(16) . . . . ? Cl1 Zn1 N1 Si1 -45.65(19) . . . . ? Cl1 Zn1 N1 Si1 -145.77(14) 2_666 . . . ? N1 Zn1 Cl1 Zn1 -115.46(11) . . . 2_666 ? Cl2 Zn1 Cl1 Zn1 109.47(5) . . . 2_666 ? Cl1 Zn1 Cl1 Zn1 0.0 2_666 . . 2_666 ? N1 P1 C1 C6 -79.5(4) . . . . ? C16 P1 C1 C6 43.1(4) . . . . ? C7 P1 C1 C6 156.2(3) . . . . ? N1 P1 C1 C2 98.8(3) . . . . ? C16 P1 C1 C2 -138.7(3) . . . . ? C7 P1 C1 C2 -25.6(4) . . . . ? C6 C1 C2 C3 0.0(6) . . . . ? P1 C1 C2 C3 -178.3(3) . . . . ? C1 C2 C3 C4 0.4(6) . . . . ? C2 C3 C4 C5 -0.7(6) . . . . ? C3 C4 C5 C6 0.5(7) . . . . ? C4 C5 C6 C1 -0.1(6) . . . . ? C2 C1 C6 C5 -0.2(6) . . . . ? P1 C1 C6 C5 178.1(3) . . . . ? N1 P1 C7 C12 162.6(3) . . . . ? C16 P1 C7 C12 41.3(3) . . . . ? C1 P1 C7 C12 -71.3(3) . . . . ? N1 P1 C7 C8 -18.2(4) . . . . ? C16 P1 C7 C8 -139.5(3) . . . . ? C1 P1 C7 C8 107.9(3) . . . . ? C12 C7 C8 C9 -0.5(6) . . . . ? P1 C7 C8 C9 -179.8(3) . . . . ? C7 C8 C9 C10 0.0(6) . . . . ? C8 C9 C10 C11 -0.1(6) . . . . ? C9 C10 C11 C12 0.7(6) . . . . ? C10 C11 C12 C7 -1.3(6) . . . . ? C8 C7 C12 C11 1.2(5) . . . . ? P1 C7 C12 C11 -179.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 0.765 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.098 #===END data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 775391' #TrackingRef 'cif_complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H22 Al Cl3 N P Si' _chemical_formula_weight 420.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.7388(13) _cell_length_b 14.3203(19) _cell_length_c 14.5442(19) _cell_angle_alpha 90.00 _cell_angle_beta 94.085(4) _cell_angle_gamma 90.00 _cell_volume 2023.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.633 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8477 _exptl_absorpt_correction_T_max 0.9055 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3390 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -3 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2247 _reflns_number_gt 2041 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0808P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2247 _refine_ls_number_parameters 212 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.1110 _refine_ls_wR_factor_gt 0.1087 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.99397(9) 0.76325(6) 0.14105(6) 0.0170(3) Uani 1 1 d . . . N1 N 0.8970(2) 0.74523(16) 0.02634(15) 0.0144(6) Uani 1 1 d . . . Cl1 Cl 0.85187(7) 0.77787(5) 0.24569(4) 0.0201(2) Uani 1 1 d . . . Cl2 Cl 1.11429(7) 0.64310(6) 0.18084(5) 0.0241(2) Uani 1 1 d . . . Cl3 Cl 1.12068(7) 0.88440(6) 0.14019(5) 0.0306(3) Uani 1 1 d . . . P1 P 0.73038(7) 0.74975(5) 0.01849(5) 0.0160(3) Uani 1 1 d . . . Si1 Si 0.99186(8) 0.71737(6) -0.07073(5) 0.0219(3) Uani 1 1 d . . . C1 C 0.6584(3) 0.7520(2) -0.0977(2) 0.0229(8) Uani 1 1 d . . . H1A H 0.6879 0.8089 -0.1281 0.034 Uiso 1 1 calc R . . H1B H 0.5577 0.7510 -0.0983 0.034 Uiso 1 1 calc R . . H1C H 0.6899 0.6972 -0.1307 0.034 Uiso 1 1 calc R . . C2 C 0.6541(3) 0.6507(2) 0.07096(19) 0.0181(8) Uani 1 1 d . . . C3 C 0.5110(3) 0.6382(2) 0.0616(2) 0.0229(8) Uani 1 1 d . . . H3 H 0.4543 0.6813 0.0267 0.027 Uiso 1 1 calc R . . C4 C 0.4535(3) 0.5628(2) 0.1035(2) 0.0264(9) Uani 1 1 d . . . H4 H 0.3564 0.5547 0.0981 0.032 Uiso 1 1 calc R . . C5 C 0.5342(3) 0.4991(2) 0.1528(2) 0.0246(8) Uani 1 1 d . . . H5 H 0.4929 0.4476 0.1814 0.030 Uiso 1 1 calc R . . C6 C 0.6761(3) 0.5101(2) 0.1610(2) 0.0249(8) Uani 1 1 d . . . H6 H 0.7322 0.4661 0.1949 0.030 Uiso 1 1 calc R . . C7 C 0.7353(3) 0.5854(2) 0.11950(19) 0.0196(7) Uani 1 1 d . . . H7 H 0.8325 0.5924 0.1243 0.024 Uiso 1 1 calc R . . C8 C 0.6721(3) 0.8582(2) 0.06525(19) 0.0175(7) Uani 1 1 d . . . C9 C 0.5531(3) 0.8659(2) 0.1129(2) 0.0239(8) Uani 1 1 d . . . H9 H 0.5013 0.8117 0.1254 0.029 Uiso 1 1 calc R . . C10 C 0.5113(3) 0.9521(2) 0.1416(2) 0.0254(8) Uani 1 1 d . . . H10 H 0.4289 0.9574 0.1725 0.030 Uiso 1 1 calc R . . C11 C 0.5873(3) 1.0308(2) 0.1261(2) 0.0298(9) Uani 1 1 d . . . H11 H 0.5586 1.0899 0.1474 0.036 Uiso 1 1 calc R . . C12 C 0.7064(3) 1.0235(2) 0.0791(2) 0.0316(9) Uani 1 1 d . . . H12 H 0.7595 1.0775 0.0686 0.038 Uiso 1 1 calc R . . C13 C 0.7469(3) 0.9378(2) 0.0481(2) 0.0254(8) Uani 1 1 d . . . H13 H 0.8269 0.9332 0.0146 0.030 Uiso 1 1 calc R . . C14 C 0.9399(4) 0.6000(3) -0.1139(3) 0.0465(12) Uani 1 1 d . . . H14A H 0.9330 0.5575 -0.0617 0.070 Uiso 1 1 calc R . . H14B H 1.0087 0.5763 -0.1540 0.070 Uiso 1 1 calc R . . H14C H 0.8503 0.6041 -0.1489 0.070 Uiso 1 1 calc R . . C15 C 0.9708(3) 0.8078(3) -0.1618(2) 0.0389(10) Uani 1 1 d . . . H15A H 0.8809 0.8003 -0.1957 0.058 Uiso 1 1 calc R . . H15B H 1.0438 0.8009 -0.2043 0.058 Uiso 1 1 calc R . . H15C H 0.9766 0.8698 -0.1334 0.058 Uiso 1 1 calc R . . C16 C 1.1773(3) 0.7103(3) -0.0337(2) 0.0262(8) Uani 1 1 d . . . H16A H 1.2038 0.7646 0.0044 0.039 Uiso 1 1 calc R . . H16B H 1.2311 0.7093 -0.0881 0.039 Uiso 1 1 calc R . . H16C H 1.1951 0.6531 0.0021 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0128(5) 0.0236(6) 0.0153(4) -0.0017(4) 0.0051(4) -0.0007(4) N1 0.0080(12) 0.0195(15) 0.0158(11) 0.0018(10) 0.0014(11) 0.0002(11) Cl1 0.0160(4) 0.0285(5) 0.0167(4) -0.0018(3) 0.0070(4) 0.0014(3) Cl2 0.0182(4) 0.0342(5) 0.0202(4) -0.0004(3) 0.0040(4) 0.0072(4) Cl3 0.0240(4) 0.0353(5) 0.0338(4) -0.0072(3) 0.0110(4) -0.0118(4) P1 0.0112(5) 0.0214(5) 0.0157(4) 0.0008(3) 0.0030(4) 0.0006(3) Si1 0.0163(5) 0.0350(6) 0.0153(4) -0.0016(3) 0.0067(4) 0.0010(4) C1 0.0138(16) 0.037(2) 0.0169(14) 0.0002(13) -0.0040(14) 0.0029(15) C2 0.0145(15) 0.0218(18) 0.0186(14) -0.0012(12) 0.0054(14) 0.0000(14) C3 0.0118(15) 0.027(2) 0.0292(16) 0.0010(13) -0.0003(15) 0.0022(15) C4 0.0154(16) 0.028(2) 0.0363(17) -0.0008(15) 0.0090(16) -0.0029(15) C5 0.0208(15) 0.0271(19) 0.0271(16) 0.0011(14) 0.0086(15) -0.0032(16) C6 0.0247(16) 0.025(2) 0.0247(14) 0.0043(13) 0.0034(15) 0.0031(16) C7 0.0121(15) 0.0221(18) 0.0245(14) -0.0020(13) 0.0008(14) 0.0005(15) C8 0.0148(15) 0.0203(18) 0.0176(13) 0.0023(12) 0.0011(14) 0.0053(14) C9 0.0169(16) 0.033(2) 0.0227(15) 0.0023(13) 0.0044(15) 0.0001(15) C10 0.0195(16) 0.033(2) 0.0239(15) -0.0003(14) 0.0035(15) 0.0098(16) C11 0.0308(18) 0.026(2) 0.0323(17) -0.0036(14) 0.0017(17) 0.0116(17) C12 0.0331(19) 0.020(2) 0.0428(18) 0.0025(15) 0.0078(18) 0.0008(17) C13 0.0177(16) 0.028(2) 0.0314(16) 0.0019(14) 0.0067(15) 0.0006(15) C14 0.036(2) 0.056(3) 0.050(2) -0.032(2) 0.016(2) -0.005(2) C15 0.0225(17) 0.068(3) 0.0265(17) 0.0204(18) 0.0077(16) 0.0059(19) C16 0.0183(16) 0.040(2) 0.0214(15) 0.0009(14) 0.0112(15) 0.0045(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 N1 1.875(3) . ? Al1 Cl3 2.1296(12) . ? Al1 Cl2 2.1381(12) . ? Al1 Cl1 2.1389(8) . ? N1 P1 1.620(2) . ? N1 Si1 1.7863(19) . ? P1 C1 1.784(3) . ? P1 C2 1.797(3) . ? P1 C8 1.803(3) . ? Si1 C16 1.850(3) . ? Si1 C15 1.853(3) . ? Si1 C14 1.852(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C7 1.385(4) . ? C2 C3 1.402(4) . ? C3 C4 1.379(4) . ? C3 H3 0.9500 . ? C4 C5 1.373(5) . ? C4 H4 0.9500 . ? C5 C6 1.388(4) . ? C5 H5 0.9500 . ? C6 C7 1.381(4) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C13 1.386(4) . ? C8 C9 1.396(3) . ? C9 C10 1.374(4) . ? C9 H9 0.9500 . ? C10 C11 1.376(5) . ? C10 H10 0.9500 . ? C11 C12 1.391(4) . ? C11 H11 0.9500 . ? C12 C13 1.375(5) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Al1 Cl3 111.22(8) . . ? N1 Al1 Cl2 111.20(9) . . ? Cl3 Al1 Cl2 110.52(5) . . ? N1 Al1 Cl1 109.65(7) . . ? Cl3 Al1 Cl1 109.21(4) . . ? Cl2 Al1 Cl1 104.83(4) . . ? P1 N1 Si1 121.66(15) . . ? P1 N1 Al1 119.70(11) . . ? Si1 N1 Al1 118.56(12) . . ? N1 P1 C1 113.07(12) . . ? N1 P1 C2 112.39(13) . . ? C1 P1 C2 105.68(15) . . ? N1 P1 C8 110.40(13) . . ? C1 P1 C8 103.22(15) . . ? C2 P1 C8 111.66(12) . . ? N1 Si1 C16 109.34(12) . . ? N1 Si1 C15 111.82(13) . . ? C16 Si1 C15 107.61(14) . . ? N1 Si1 C14 109.06(13) . . ? C16 Si1 C14 106.64(17) . . ? C15 Si1 C14 112.2(2) . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 C3 119.4(3) . . ? C7 C2 P1 120.8(2) . . ? C3 C2 P1 119.8(2) . . ? C4 C3 C2 119.3(3) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C5 C4 C3 121.1(3) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 C6 119.9(3) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C7 C6 C5 119.7(3) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C2 C7 C6 120.6(3) . . ? C2 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C13 C8 C9 119.4(3) . . ? C13 C8 P1 117.19(18) . . ? C9 C8 P1 123.4(2) . . ? C10 C9 C8 119.8(3) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C9 120.8(2) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 119.7(3) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C13 C12 C11 119.8(3) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C8 120.5(2) . . ? C12 C13 H13 119.7 . . ? C8 C13 H13 119.7 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.630 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.630 _refine_diff_density_max 0.426 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.070 #===END data_complex_5 _database_code_depnum_ccdc_archive 'CCDC 775392' #TrackingRef 'cif_complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H84 Cl2 N4 O P4 Si4 Zn4' _chemical_formula_weight 1493.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P-42(1)c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 14.8254(19) _cell_length_b 14.8254(19) _cell_length_c 16.278(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3577.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description hexagonal _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1548 _exptl_absorpt_coefficient_mu 1.597 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7619 _exptl_absorpt_correction_T_max 0.8439 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12415 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0808 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3156 _reflns_number_gt 2620 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.000(14) _refine_ls_number_reflns 3156 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0456 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0581 _refine_ls_wR_factor_gt 0.0570 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn2 Zn -0.02993(3) 0.09963(3) 0.07541(3) 0.01899(13) Uani 1 1 d . . . Cl22 Cl 0.0000 0.0000 0.19475(11) 0.0369(5) Uani 1 2 d S . . N3 N 0.0657(2) 0.1965(2) 0.0970(2) 0.0173(9) Uani 1 1 d . . . O1 O 0.0000 0.0000 0.0000 0.0177(14) Uani 1 4 d S . . P4 P 0.15587(7) 0.19530(7) 0.04307(7) 0.0174(3) Uani 1 1 d . . . Si18 Si 0.04637(8) 0.26671(8) 0.18115(8) 0.0243(3) Uani 1 1 d . . . C5 C -0.1610(2) 0.1381(3) 0.0575(3) 0.0212(11) Uani 1 1 d . . . H5A H -0.2005 0.0912 0.0817 0.025 Uiso 1 1 calc R . . H5B H -0.1714 0.1945 0.0886 0.025 Uiso 1 1 calc R . . C6 C 0.2414(3) 0.1207(2) 0.0856(3) 0.0165(10) Uani 1 1 d . . . C7 C 0.3228(3) 0.1103(3) 0.0464(3) 0.0287(12) Uani 1 1 d . . . H7 H 0.3332 0.1393 -0.0048 0.034 Uiso 1 1 calc R . . C8 C 0.3903(3) 0.0572(3) 0.0814(3) 0.0337(12) Uani 1 1 d . . . H8 H 0.4471 0.0519 0.0549 0.040 Uiso 1 1 calc R . . C9 C 0.3753(3) 0.0131(3) 0.1531(3) 0.0311(13) Uani 1 1 d . . . H9 H 0.4213 -0.0240 0.1757 0.037 Uiso 1 1 calc R . . C10 C 0.2943(3) 0.0214(3) 0.1932(3) 0.0291(12) Uani 1 1 d . . . H10 H 0.2841 -0.0093 0.2436 0.035 Uiso 1 1 calc R . . C11 C 0.2275(3) 0.0754(3) 0.1592(3) 0.0248(12) Uani 1 1 d . . . H11 H 0.1713 0.0814 0.1866 0.030 Uiso 1 1 calc R . . C12 C 0.2141(3) 0.3041(3) 0.0449(3) 0.0176(10) Uani 1 1 d . . . C13 C 0.1915(3) 0.3685(3) -0.0132(3) 0.0275(12) Uani 1 1 d . . . H13 H 0.1457 0.3555 -0.0523 0.033 Uiso 1 1 calc R . . C14 C 0.2349(3) 0.4524(3) -0.0154(3) 0.0331(13) Uani 1 1 d . . . H14 H 0.2197 0.4957 -0.0562 0.040 Uiso 1 1 calc R . . C15 C 0.3000(3) 0.4709(3) 0.0428(3) 0.0371(13) Uani 1 1 d . . . H15 H 0.3288 0.5281 0.0428 0.045 Uiso 1 1 calc R . . C16 C 0.3238(3) 0.4086(3) 0.1002(3) 0.0352(13) Uani 1 1 d . . . H16 H 0.3690 0.4223 0.1395 0.042 Uiso 1 1 calc R . . C17 C 0.2816(3) 0.3246(3) 0.1011(3) 0.0269(12) Uani 1 1 d . . . H17 H 0.2991 0.2809 0.1407 0.032 Uiso 1 1 calc R . . C19 C 0.0412(3) 0.3876(3) 0.1507(3) 0.0423(14) Uani 1 1 d . . . H19A H 0.1025 0.4108 0.1432 0.064 Uiso 1 1 calc R . . H19B H 0.0107 0.4222 0.1938 0.064 Uiso 1 1 calc R . . H19C H 0.0077 0.3934 0.0991 0.064 Uiso 1 1 calc R . . C20 C 0.1313(3) 0.2529(3) 0.2641(3) 0.0420(15) Uani 1 1 d . . . H20A H 0.1252 0.1928 0.2886 0.063 Uiso 1 1 calc R . . H20B H 0.1215 0.2989 0.3064 0.063 Uiso 1 1 calc R . . H20C H 0.1920 0.2596 0.2411 0.063 Uiso 1 1 calc R . . C21 C -0.0638(3) 0.2420(3) 0.2303(3) 0.0434(15) Uani 1 1 d . . . H21A H -0.1127 0.2625 0.1944 0.065 Uiso 1 1 calc R . . H21B H -0.0675 0.2734 0.2831 0.065 Uiso 1 1 calc R . . H21C H -0.0693 0.1768 0.2393 0.065 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn2 0.0144(3) 0.0183(3) 0.0242(3) -0.0003(3) -0.0003(3) -0.0008(2) Cl22 0.0322(11) 0.0318(11) 0.0468(12) 0.000 0.000 -0.0039(8) N3 0.0158(19) 0.0149(19) 0.021(2) 0.0001(16) -0.0046(16) 0.0030(15) O1 0.012(2) 0.012(2) 0.029(4) 0.000 0.000 0.000 P4 0.0161(6) 0.0133(6) 0.0229(7) 0.0017(5) -0.0010(6) 0.0004(5) Si18 0.0217(8) 0.0241(8) 0.0271(8) -0.0068(6) 0.0014(6) -0.0007(6) C5 0.018(2) 0.016(2) 0.030(3) -0.002(2) 0.006(2) 0.000(2) C6 0.016(2) 0.012(2) 0.021(3) 0.000(2) -0.005(2) -0.0068(18) C7 0.035(3) 0.023(3) 0.029(3) 0.004(2) -0.001(2) 0.006(2) C8 0.021(3) 0.029(3) 0.051(3) 0.005(3) 0.000(3) 0.011(2) C9 0.028(3) 0.020(3) 0.045(3) 0.005(3) -0.014(3) 0.004(2) C10 0.029(3) 0.024(3) 0.035(3) 0.008(2) -0.013(3) -0.004(2) C11 0.019(3) 0.019(3) 0.036(3) -0.007(2) -0.003(2) -0.003(2) C12 0.013(2) 0.017(2) 0.023(3) -0.001(2) 0.001(2) 0.0025(19) C13 0.025(3) 0.019(3) 0.039(3) -0.003(2) -0.005(2) 0.001(2) C14 0.041(3) 0.015(3) 0.043(4) 0.012(2) -0.003(3) -0.004(2) C15 0.039(3) 0.019(3) 0.053(4) -0.001(3) -0.002(3) -0.012(3) C16 0.027(3) 0.029(3) 0.049(4) -0.003(3) -0.009(3) -0.009(2) C17 0.024(3) 0.020(3) 0.037(3) -0.001(2) -0.006(2) 0.002(2) C19 0.053(4) 0.033(3) 0.042(3) -0.014(3) -0.001(3) 0.011(3) C20 0.048(4) 0.042(3) 0.036(4) -0.014(3) 0.005(3) 0.002(3) C21 0.042(3) 0.046(4) 0.042(4) -0.024(3) 0.017(3) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn2 O1 1.9712(5) . ? Zn2 C5 2.047(4) . ? Zn2 N3 2.048(3) . ? Zn2 Cl22 2.4803(15) . ? Zn2 Zn2 3.0845(10) 2 ? Cl22 Zn2 2.4803(15) 2 ? N3 P4 1.600(3) . ? N3 Si18 1.744(3) . ? O1 Zn2 1.9712(5) 4 ? O1 Zn2 1.9712(5) 2 ? O1 Zn2 1.9712(5) 3 ? P4 C5 1.734(4) 3 ? P4 C6 1.820(4) . ? P4 C12 1.830(4) . ? Si18 C21 1.854(4) . ? Si18 C20 1.858(5) . ? Si18 C19 1.861(4) . ? C5 P4 1.734(4) 4 ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.374(5) . ? C6 C11 1.388(6) . ? C7 C8 1.395(5) . ? C7 H7 0.9500 . ? C8 C9 1.356(6) . ? C8 H8 0.9500 . ? C9 C10 1.373(5) . ? C9 H9 0.9500 . ? C10 C11 1.389(5) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.385(5) . ? C12 C17 1.390(5) . ? C13 C14 1.400(5) . ? C13 H13 0.9500 . ? C14 C15 1.381(6) . ? C14 H14 0.9500 . ? C15 C16 1.359(6) . ? C15 H15 0.9500 . ? C16 C17 1.393(5) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn2 C5 109.48(12) . . ? O1 Zn2 N3 118.46(9) . . ? C5 Zn2 N3 119.10(14) . . ? O1 Zn2 Cl22 90.07(3) . . ? C5 Zn2 Cl22 116.58(12) . . ? N3 Zn2 Cl22 99.18(9) . . ? O1 Zn2 Zn2 38.519(16) . 2 ? C5 Zn2 Zn2 122.68(11) . 2 ? N3 Zn2 Zn2 118.20(8) . 2 ? Cl22 Zn2 Zn2 51.55(3) . 2 ? Zn2 Cl22 Zn2 76.90(6) 2 . ? P4 N3 Si18 125.08(19) . . ? P4 N3 Zn2 118.45(18) . . ? Si18 N3 Zn2 116.09(17) . . ? Zn2 O1 Zn2 112.821(17) 4 . ? Zn2 O1 Zn2 112.821(17) 4 2 ? Zn2 O1 Zn2 102.96(3) . 2 ? Zn2 O1 Zn2 102.96(3) 4 3 ? Zn2 O1 Zn2 112.821(17) . 3 ? Zn2 O1 Zn2 112.821(17) 2 3 ? N3 P4 C5 113.20(18) . 3 ? N3 P4 C6 112.39(19) . . ? C5 P4 C6 106.7(2) 3 . ? N3 P4 C12 112.07(17) . . ? C5 P4 C12 110.19(19) 3 . ? C6 P4 C12 101.57(17) . . ? N3 Si18 C21 111.40(18) . . ? N3 Si18 C20 113.21(19) . . ? C21 Si18 C20 105.2(2) . . ? N3 Si18 C19 111.86(19) . . ? C21 Si18 C19 105.6(2) . . ? C20 Si18 C19 109.1(2) . . ? P4 C5 Zn2 117.1(2) 4 . ? P4 C5 H5A 108.0 4 . ? Zn2 C5 H5A 108.0 . . ? P4 C5 H5B 108.0 4 . ? Zn2 C5 H5B 108.0 . . ? H5A C5 H5B 107.3 . . ? C7 C6 C11 118.5(4) . . ? C7 C6 P4 120.3(3) . . ? C11 C6 P4 121.2(3) . . ? C6 C7 C8 120.2(4) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C9 C8 C7 120.4(4) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 120.7(4) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C9 C10 C11 119.0(4) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C10 C11 C6 121.1(4) . . ? C10 C11 H11 119.4 . . ? C6 C11 H11 119.4 . . ? C13 C12 C17 118.2(4) . . ? C13 C12 P4 118.8(3) . . ? C17 C12 P4 122.9(3) . . ? C12 C13 C14 121.2(4) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C15 C14 C13 118.7(4) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C16 C15 C14 121.1(4) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C17 119.9(4) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C12 C17 C16 120.8(4) . . ? C12 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? Si18 C19 H19A 109.5 . . ? Si18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si18 C20 H20A 109.5 . . ? Si18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si18 C21 H21A 109.5 . . ? Si18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Zn2 Cl22 Zn2 0.0 . . . 2 ? C5 Zn2 Cl22 Zn2 111.93(13) . . . 2 ? N3 Zn2 Cl22 Zn2 -118.88(9) . . . 2 ? O1 Zn2 N3 P4 8.0(2) . . . . ? C5 Zn2 N3 P4 -129.4(2) . . . . ? Cl22 Zn2 N3 P4 103.14(18) . . . . ? Zn2 Zn2 N3 P4 52.0(2) 2 . . . ? O1 Zn2 N3 Si18 -165.28(12) . . . . ? C5 Zn2 N3 Si18 57.3(2) . . . . ? Cl22 Zn2 N3 Si18 -70.17(16) . . . . ? Zn2 Zn2 N3 Si18 -121.27(14) 2 . . . ? C5 Zn2 O1 Zn2 3.55(12) . . . 4 ? N3 Zn2 O1 Zn2 -137.59(10) . . . 4 ? Cl22 Zn2 O1 Zn2 121.914(9) . . . 4 ? Zn2 Zn2 O1 Zn2 121.914(9) 2 . . 4 ? C5 Zn2 O1 Zn2 -118.37(12) . . . 2 ? N3 Zn2 O1 Zn2 100.50(10) . . . 2 ? Cl22 Zn2 O1 Zn2 0.0 . . . 2 ? C5 Zn2 O1 Zn2 119.72(12) . . . 3 ? N3 Zn2 O1 Zn2 -21.42(10) . . . 3 ? Cl22 Zn2 O1 Zn2 -121.914(9) . . . 3 ? Zn2 Zn2 O1 Zn2 -121.914(9) 2 . . 3 ? Si18 N3 P4 C5 -152.1(2) . . . 3 ? Zn2 N3 P4 C5 35.2(2) . . . 3 ? Si18 N3 P4 C6 86.9(3) . . . . ? Zn2 N3 P4 C6 -85.8(2) . . . . ? Si18 N3 P4 C12 -26.7(3) . . . . ? Zn2 N3 P4 C12 160.59(19) . . . . ? P4 N3 Si18 C21 -176.5(2) . . . . ? Zn2 N3 Si18 C21 -3.7(3) . . . . ? P4 N3 Si18 C20 -58.3(3) . . . . ? Zn2 N3 Si18 C20 114.6(2) . . . . ? P4 N3 Si18 C19 65.5(3) . . . . ? Zn2 N3 Si18 C19 -121.7(2) . . . . ? O1 Zn2 C5 P4 -48.2(2) . . . 4 ? N3 Zn2 C5 P4 92.7(2) . . . 4 ? Cl22 Zn2 C5 P4 -148.46(16) . . . 4 ? Zn2 Zn2 C5 P4 -88.8(2) 2 . . 4 ? N3 P4 C6 C7 179.0(3) . . . . ? C5 P4 C6 C7 54.3(4) 3 . . . ? C12 P4 C6 C7 -61.1(4) . . . . ? N3 P4 C6 C11 -3.0(4) . . . . ? C5 P4 C6 C11 -127.7(4) 3 . . . ? C12 P4 C6 C11 116.9(3) . . . . ? C11 C6 C7 C8 -1.7(6) . . . . ? P4 C6 C7 C8 176.3(3) . . . . ? C6 C7 C8 C9 2.1(7) . . . . ? C7 C8 C9 C10 -1.4(7) . . . . ? C8 C9 C10 C11 0.4(7) . . . . ? C9 C10 C11 C6 0.0(6) . . . . ? C7 C6 C11 C10 0.7(6) . . . . ? P4 C6 C11 C10 -177.3(3) . . . . ? N3 P4 C12 C13 -88.8(4) . . . . ? C5 P4 C12 C13 38.2(4) 3 . . . ? C6 P4 C12 C13 151.0(3) . . . . ? N3 P4 C12 C17 92.5(4) . . . . ? C5 P4 C12 C17 -140.5(4) 3 . . . ? C6 P4 C12 C17 -27.7(4) . . . . ? C17 C12 C13 C14 -0.3(6) . . . . ? P4 C12 C13 C14 -179.1(3) . . . . ? C12 C13 C14 C15 -1.2(7) . . . . ? C13 C14 C15 C16 1.6(7) . . . . ? C14 C15 C16 C17 -0.5(7) . . . . ? C13 C12 C17 C16 1.4(6) . . . . ? P4 C12 C17 C16 -179.8(3) . . . . ? C15 C16 C17 C12 -1.1(7) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.690 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.071 #===END data_complex_6 _database_code_depnum_ccdc_archive 'CCDC 775393' #TrackingRef 'cif_complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H84 Cl2 Mg4 N4 O P4 Si4' _chemical_formula_weight 1329.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P-42(1)c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 14.8622(16) _cell_length_b 14.8622(16) _cell_length_c 16.258(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3591.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description hexagonal _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1404 _exptl_absorpt_coefficient_mu 0.323 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9324 _exptl_absorpt_correction_T_max 0.9562 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9585 _diffrn_reflns_av_R_equivalents 0.0849 _diffrn_reflns_av_sigmaI/netI 0.0626 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 24.97 _reflns_number_total 2704 _reflns_number_gt 2452 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(14) _refine_ls_number_reflns 2704 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.0957 _refine_ls_wR_factor_gt 0.0939 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl22 Cl 1.0000 1.0000 0.80525(9) 0.0260(3) Uani 1 2 d S . . P4 P 0.83939(6) 0.80036(5) 0.95563(7) 0.0213(3) Uani 1 1 d . . . Si18 Si 0.94865(7) 0.72975(7) 0.81738(8) 0.0315(3) Uani 1 1 d . . . Mg2 Mg 1.02314(7) 0.89998(7) 0.92435(7) 0.0201(3) Uani 1 1 d . . . C6 C 0.7540(2) 0.8745(2) 0.9137(3) 0.0251(9) Uani 1 1 d . . . C12 C 0.7811(2) 0.6914(2) 0.9540(2) 0.0252(9) Uani 1 1 d . . . C10 C 0.7029(2) 0.9773(2) 0.8092(3) 0.0371(10) Uani 1 1 d . . . H10 H 0.7132 1.0086 0.7591 0.045 Uiso 1 1 calc R . . C13 C 0.7152(2) 0.6708(3) 0.8979(3) 0.0342(10) Uani 1 1 d . . . H13 H 0.6979 0.7147 0.8585 0.041 Uiso 1 1 calc R . . C11 C 0.7687(2) 0.9220(2) 0.8413(3) 0.0299(10) Uani 1 1 d . . . H11 H 0.8247 0.9164 0.8136 0.036 Uiso 1 1 calc R . . C5 C 0.8602(2) 0.8373(2) 1.0539(3) 0.0261(9) Uani 1 1 d . . . H5A H 0.9080 0.7984 1.0771 0.031 Uiso 1 1 calc R . . H5B H 0.8051 0.8260 1.0866 0.031 Uiso 1 1 calc R . . C21 C 1.0594(3) 0.7566(3) 0.7700(3) 0.0528(13) Uani 1 1 d . . . H21A H 1.0630 0.8214 0.7591 0.079 Uiso 1 1 calc R . . H21B H 1.0659 0.7234 0.7183 0.079 Uiso 1 1 calc R . . H21C H 1.1078 0.7393 0.8078 0.079 Uiso 1 1 calc R . . C15 C 0.6960(3) 0.5249(3) 0.9542(3) 0.0478(12) Uani 1 1 d . . . H15 H 0.6678 0.4676 0.9541 0.057 Uiso 1 1 calc R . . C17 C 0.8035(2) 0.6274(2) 1.0113(3) 0.0336(10) Uani 1 1 d . . . H17 H 0.8492 0.6399 1.0506 0.040 Uiso 1 1 calc R . . C7 C 0.6725(2) 0.8849(2) 0.9536(3) 0.0348(10) Uani 1 1 d . . . H7 H 0.6616 0.8531 1.0034 0.042 Uiso 1 1 calc R . . C16 C 0.7605(3) 0.5451(3) 1.0126(3) 0.0446(12) Uani 1 1 d . . . H16 H 0.7753 0.5021 1.0537 0.054 Uiso 1 1 calc R . . C14 C 0.6732(3) 0.5872(3) 0.8972(3) 0.0428(12) Uani 1 1 d . . . H14 H 0.6287 0.5739 0.8570 0.051 Uiso 1 1 calc R . . C19 C 0.9548(3) 0.6098(3) 0.8482(3) 0.0473(12) Uani 1 1 d . . . H19A H 0.9906 0.6042 0.8986 0.071 Uiso 1 1 calc R . . H19B H 0.9832 0.5749 0.8041 0.071 Uiso 1 1 calc R . . H19C H 0.8940 0.5868 0.8581 0.071 Uiso 1 1 calc R . . C8 C 0.6075(3) 0.9404(2) 0.9223(3) 0.0402(11) Uani 1 1 d . . . H8 H 0.5518 0.9470 0.9504 0.048 Uiso 1 1 calc R . . C9 C 0.6226(2) 0.9869(2) 0.8500(3) 0.0370(11) Uani 1 1 d . . . H9 H 0.5774 1.0256 0.8286 0.044 Uiso 1 1 calc R . . N3 N 0.92935(17) 0.80013(17) 0.90035(18) 0.0221(7) Uani 1 1 d . . . C20 C 0.8636(3) 0.7413(3) 0.7342(3) 0.0500(13) Uani 1 1 d . . . H20A H 0.8030 0.7375 0.7579 0.075 Uiso 1 1 calc R . . H20B H 0.8717 0.6929 0.6940 0.075 Uiso 1 1 calc R . . H20C H 0.8710 0.7997 0.7070 0.075 Uiso 1 1 calc R . . O1 O 1.0000 1.0000 1.0000 0.0167(10) Uani 1 4 d S . . 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 Cl22 0.0313(6) 0.0279(6) 0.0187(9) 0.000 0.000 -0.0057(5) P4 0.0206(4) 0.0202(4) 0.0229(7) 0.0008(4) -0.0015(4) -0.0001(3) Si18 0.0328(5) 0.0303(5) 0.0313(9) -0.0116(5) 0.0039(5) -0.0028(4) Mg2 0.0195(5) 0.0202(5) 0.0208(9) -0.0017(5) -0.0007(5) -0.0019(4) C6 0.0272(18) 0.0225(17) 0.026(3) -0.0023(17) -0.0059(17) -0.0004(13) C12 0.0222(17) 0.0211(16) 0.032(3) 0.0032(17) 0.0003(17) -0.0005(13) C10 0.039(2) 0.0302(19) 0.042(3) 0.0125(19) -0.012(2) -0.0043(16) C13 0.032(2) 0.033(2) 0.038(3) -0.0004(19) -0.0069(19) -0.0032(15) C11 0.0264(18) 0.0313(19) 0.032(3) 0.0023(18) -0.0069(17) -0.0054(15) C5 0.0244(17) 0.0241(17) 0.030(3) -0.0057(17) -0.0068(16) 0.0027(14) C21 0.051(3) 0.063(3) 0.045(4) -0.027(2) 0.022(2) -0.015(2) C15 0.048(2) 0.032(2) 0.063(4) 0.002(2) 0.003(2) -0.0171(18) C17 0.036(2) 0.032(2) 0.032(3) 0.0009(19) -0.0058(19) -0.0028(15) C7 0.0317(19) 0.0341(19) 0.039(3) 0.0063(19) 0.0036(19) 0.0060(15) C16 0.055(3) 0.031(2) 0.048(3) 0.011(2) -0.002(2) -0.0072(18) C14 0.040(2) 0.037(2) 0.052(4) -0.003(2) -0.007(2) -0.0102(18) C19 0.060(3) 0.035(2) 0.047(3) -0.012(2) 0.004(2) 0.0077(19) C8 0.035(2) 0.038(2) 0.047(3) 0.003(2) 0.000(2) 0.0111(16) C9 0.032(2) 0.0283(19) 0.051(3) 0.001(2) -0.017(2) 0.0034(16) N3 0.0231(14) 0.0209(14) 0.022(2) -0.0047(13) -0.0013(13) -0.0039(11) C20 0.063(3) 0.062(3) 0.025(4) -0.015(2) 0.000(2) 0.004(2) O1 0.0191(13) 0.0191(13) 0.012(3) 0.000 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl22 Mg2 2.4652(16) 2_775 ? Cl22 Mg2 2.4652(16) . ? P4 N3 1.611(3) . ? P4 C5 1.717(4) . ? P4 C6 1.814(3) . ? P4 C12 1.836(3) . ? Si18 N3 1.731(3) . ? Si18 C19 1.854(4) . ? Si18 C20 1.859(5) . ? Si18 C21 1.861(4) . ? Mg2 O1 1.9598(11) . ? Mg2 N3 2.073(3) . ? Mg2 C5 2.186(3) 4_757 ? Mg2 Mg2 3.052(2) 2_775 ? Mg2 Mg2 3.272(2) 4_757 ? Mg2 Mg2 3.272(2) 3_577 ? C6 C7 1.383(5) . ? C6 C11 1.389(5) . ? C12 C13 1.373(5) . ? C12 C17 1.373(5) . ? C10 C9 1.373(6) . ? C10 C11 1.379(5) . ? C13 C14 1.390(5) . ? C5 Mg2 2.186(3) 3_577 ? C15 C14 1.353(6) . ? C15 C16 1.382(6) . ? C17 C16 1.381(5) . ? C7 C8 1.369(5) . ? C8 C9 1.382(5) . ? O1 Mg2 1.9598(11) 4_757 ? O1 Mg2 1.9598(11) 3_577 ? O1 Mg2 1.9598(11) 2_775 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Mg2 Cl22 Mg2 76.48(6) 2_775 . ? N3 P4 C5 111.75(16) . . ? N3 P4 C6 111.82(17) . . ? C5 P4 C6 106.36(17) . . ? N3 P4 C12 112.44(15) . . ? C5 P4 C12 112.32(18) . . ? C6 P4 C12 101.56(15) . . ? N3 Si18 C19 112.27(18) . . ? N3 Si18 C20 113.44(17) . . ? C19 Si18 C20 108.6(2) . . ? N3 Si18 C21 109.82(17) . . ? C19 Si18 C21 105.9(2) . . ? C20 Si18 C21 106.3(2) . . ? O1 Mg2 N3 122.90(9) . . ? O1 Mg2 C5 105.68(11) . 4_757 ? N3 Mg2 C5 118.35(12) . 4_757 ? O1 Mg2 Cl22 90.63(4) . . ? N3 Mg2 Cl22 100.95(9) . . ? C5 Mg2 Cl22 115.00(11) 4_757 . ? O1 Mg2 Mg2 38.87(3) . 2_775 ? N3 Mg2 Mg2 123.09(9) . 2_775 ? C5 Mg2 Mg2 118.53(10) 4_757 2_775 ? Cl22 Mg2 Mg2 51.76(3) . 2_775 ? O1 Mg2 Mg2 33.403(18) . 4_757 ? N3 Mg2 Mg2 140.96(10) . 4_757 ? C5 Mg2 Mg2 72.45(11) 4_757 4_757 ? Cl22 Mg2 Mg2 107.57(4) . 4_757 ? Mg2 Mg2 Mg2 62.21(2) 2_775 4_757 ? O1 Mg2 Mg2 33.403(18) . 3_577 ? N3 Mg2 Mg2 90.88(9) . 3_577 ? C5 Mg2 Mg2 120.25(13) 4_757 3_577 ? Cl22 Mg2 Mg2 107.57(4) . 3_577 ? Mg2 Mg2 Mg2 62.21(2) 2_775 3_577 ? Mg2 Mg2 Mg2 55.59(4) 4_757 3_577 ? C7 C6 C11 118.6(3) . . ? C7 C6 P4 120.2(3) . . ? C11 C6 P4 121.2(3) . . ? C13 C12 C17 118.0(3) . . ? C13 C12 P4 122.9(3) . . ? C17 C12 P4 119.1(3) . . ? C9 C10 C11 119.7(4) . . ? C12 C13 C14 121.7(4) . . ? C10 C11 C6 120.8(4) . . ? P4 C5 Mg2 120.2(2) . 3_577 ? C14 C15 C16 119.8(4) . . ? C12 C17 C16 120.8(4) . . ? C8 C7 C6 120.7(4) . . ? C17 C16 C15 120.2(4) . . ? C15 C14 C13 119.5(4) . . ? C7 C8 C9 120.2(4) . . ? C10 C9 C8 120.0(4) . . ? P4 N3 Si18 125.00(16) . . ? P4 N3 Mg2 116.84(15) . . ? Si18 N3 Mg2 117.89(15) . . ? Mg2 O1 Mg2 102.26(7) 4_757 3_577 ? Mg2 O1 Mg2 113.19(4) 4_757 . ? Mg2 O1 Mg2 113.19(4) 3_577 . ? Mg2 O1 Mg2 113.19(4) 4_757 2_775 ? Mg2 O1 Mg2 113.19(4) 3_577 2_775 ? Mg2 O1 Mg2 102.26(7) . 2_775 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Mg2 Cl22 Mg2 O1 0.0 2_775 . . . ? Mg2 Cl22 Mg2 N3 123.74(9) 2_775 . . . ? Mg2 Cl22 Mg2 C5 -107.66(12) 2_775 . . 4_757 ? Mg2 Cl22 Mg2 Mg2 -29.282(18) 2_775 . . 4_757 ? Mg2 Cl22 Mg2 Mg2 29.282(18) 2_775 . . 3_577 ? N3 P4 C6 C7 -178.8(3) . . . . ? C5 P4 C6 C7 -56.6(3) . . . . ? C12 P4 C6 C7 61.1(3) . . . . ? N3 P4 C6 C11 1.1(3) . . . . ? C5 P4 C6 C11 123.4(3) . . . . ? C12 P4 C6 C11 -119.0(3) . . . . ? N3 P4 C12 C13 -91.0(3) . . . . ? C5 P4 C12 C13 141.9(3) . . . . ? C6 P4 C12 C13 28.7(4) . . . . ? N3 P4 C12 C17 89.3(3) . . . . ? C5 P4 C12 C17 -37.8(3) . . . . ? C6 P4 C12 C17 -151.0(3) . . . . ? C17 C12 C13 C14 -1.3(6) . . . . ? P4 C12 C13 C14 178.9(3) . . . . ? C9 C10 C11 C6 1.3(6) . . . . ? C7 C6 C11 C10 -1.0(5) . . . . ? P4 C6 C11 C10 179.1(3) . . . . ? N3 P4 C5 Mg2 66.6(2) . . . 3_577 ? C6 P4 C5 Mg2 -55.7(2) . . . 3_577 ? C12 P4 C5 Mg2 -165.92(16) . . . 3_577 ? C13 C12 C17 C16 -0.4(6) . . . . ? P4 C12 C17 C16 179.3(3) . . . . ? C11 C6 C7 C8 0.3(6) . . . . ? P4 C6 C7 C8 -179.7(3) . . . . ? C12 C17 C16 C15 2.0(6) . . . . ? C14 C15 C16 C17 -1.9(7) . . . . ? C16 C15 C14 C13 0.2(7) . . . . ? C12 C13 C14 C15 1.5(6) . . . . ? C6 C7 C8 C9 0.0(6) . . . . ? C11 C10 C9 C8 -0.9(6) . . . . ? C7 C8 C9 C10 0.2(6) . . . . ? C5 P4 N3 Si18 152.6(2) . . . . ? C6 P4 N3 Si18 -88.3(2) . . . . ? C12 P4 N3 Si18 25.3(3) . . . . ? C5 P4 N3 Mg2 -33.4(2) . . . . ? C6 P4 N3 Mg2 85.7(2) . . . . ? C12 P4 N3 Mg2 -160.77(17) . . . . ? C19 Si18 N3 P4 -64.6(3) . . . . ? C20 Si18 N3 P4 59.0(3) . . . . ? C21 Si18 N3 P4 177.8(2) . . . . ? C19 Si18 N3 Mg2 121.46(19) . . . . ? C20 Si18 N3 Mg2 -114.9(2) . . . . ? C21 Si18 N3 Mg2 3.9(3) . . . . ? O1 Mg2 N3 P4 -7.6(2) . . . . ? C5 Mg2 N3 P4 128.00(19) 4_757 . . . ? Cl22 Mg2 N3 P4 -105.59(16) . . . . ? Mg2 Mg2 N3 P4 -54.4(2) 2_775 . . . ? Mg2 Mg2 N3 P4 31.0(2) 4_757 . . . ? Mg2 Mg2 N3 P4 2.50(16) 3_577 . . . ? O1 Mg2 N3 Si18 166.80(11) . . . . ? C5 Mg2 N3 Si18 -57.6(2) 4_757 . . . ? Cl22 Mg2 N3 Si18 68.83(16) . . . . ? Mg2 Mg2 N3 Si18 120.05(13) 2_775 . . . ? Mg2 Mg2 N3 Si18 -154.55(10) 4_757 . . . ? Mg2 Mg2 N3 Si18 176.92(15) 3_577 . . . ? N3 Mg2 O1 Mg2 134.39(13) . . . 4_757 ? C5 Mg2 O1 Mg2 -5.87(11) 4_757 . . 4_757 ? Cl22 Mg2 O1 Mg2 -122.111(19) . . . 4_757 ? Mg2 Mg2 O1 Mg2 -122.111(19) 2_775 . . 4_757 ? Mg2 Mg2 O1 Mg2 115.78(4) 3_577 . . 4_757 ? N3 Mg2 O1 Mg2 18.61(11) . . . 3_577 ? C5 Mg2 O1 Mg2 -121.65(12) 4_757 . . 3_577 ? Cl22 Mg2 O1 Mg2 122.112(19) . . . 3_577 ? Mg2 Mg2 O1 Mg2 122.112(18) 2_775 . . 3_577 ? Mg2 Mg2 O1 Mg2 -115.78(4) 4_757 . . 3_577 ? N3 Mg2 O1 Mg2 -103.50(12) . . . 2_775 ? C5 Mg2 O1 Mg2 116.24(11) 4_757 . . 2_775 ? Cl22 Mg2 O1 Mg2 0.0 . . . 2_775 ? Mg2 Mg2 O1 Mg2 122.111(19) 4_757 . . 2_775 ? Mg2 Mg2 O1 Mg2 -122.112(18) 3_577 . . 2_775 ? _diffrn_measured_fraction_theta_max 0.869 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.869 _refine_diff_density_max 0.375 _refine_diff_density_min -0.188 _refine_diff_density_rms 0.060 #===END data_complex_7 _database_code_depnum_ccdc_archive 'CCDC 775394' #TrackingRef 'cif_complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H74 Al2 Cl4 N2 O6 P2 Si2' _chemical_formula_weight 1088.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3733(9) _cell_length_b 11.8131(12) _cell_length_c 14.4903(14) _cell_angle_alpha 114.0080(10) _cell_angle_beta 91.232(2) _cell_angle_gamma 103.912(2) _cell_volume 1409.7(2) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.283 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 0.386 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9199 _exptl_absorpt_correction_T_max 0.9479 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11567 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4930 _reflns_number_gt 4511 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1144P)^2^+1.8020P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4930 _refine_ls_number_parameters 392 _refine_ls_number_restraints 220 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1390 _refine_ls_wR_factor_gt 0.1333 _refine_ls_goodness_of_fit_ref 0.800 _refine_ls_restrained_S_all 0.791 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 1.08818(8) 0.13231(7) 0.57551(5) 0.02490(19) Uani 1 1 d . . . Cl1 Cl 1.15135(7) 0.24623(6) 0.48971(5) 0.03441(18) Uani 1 1 d . . . Cl2 Cl 1.27865(7) 0.13281(7) 0.66361(5) 0.03706(19) Uani 1 1 d . . . N1 N 1.0121(2) 0.25224(19) 0.68950(15) 0.0273(4) Uani 1 1 d . . . O1 O 0.90068(18) 0.02367(16) 0.53576(13) 0.0282(4) Uani 1 1 d . . . P1 P 0.83499(7) 0.21933(6) 0.67205(5) 0.02570(18) Uani 1 1 d . . . Si1 Si 1.12365(8) 0.38520(7) 0.79604(5) 0.0343(2) Uani 1 1 d . . . C1 C 0.7777(3) 0.0481(2) 0.5873(2) 0.0309(5) Uani 1 1 d . . . H1A H 0.7535 -0.0040 0.6267 0.037 Uiso 1 1 calc R . . H1B H 0.6897 0.0275 0.5384 0.037 Uiso 1 1 calc R . . C2 C 0.7666(3) 0.3027(2) 0.60922(19) 0.0304(5) Uani 1 1 d . . . C3 C 0.6167(3) 0.2707(3) 0.5742(2) 0.0390(6) Uani 1 1 d . . . H3 H 0.5484 0.2039 0.5840 0.047 Uiso 1 1 calc R . . C4 C 0.5668(3) 0.3356(4) 0.5254(3) 0.0517(8) Uani 1 1 d . . . H4 H 0.4643 0.3136 0.5016 0.062 Uiso 1 1 calc R . . C5 C 0.6656(4) 0.4323(4) 0.5111(3) 0.0527(8) Uani 1 1 d . . . H5 H 0.6309 0.4770 0.4778 0.063 Uiso 1 1 calc R . . C6 C 0.8147(3) 0.4644(3) 0.5451(3) 0.0466(8) Uani 1 1 d . . . H6 H 0.8824 0.5313 0.5352 0.056 Uiso 1 1 calc R . . C7 C 0.8656(3) 0.3993(3) 0.5936(2) 0.0354(6) Uani 1 1 d . . . H7 H 0.9685 0.4207 0.6163 0.042 Uiso 1 1 calc R . . C8 C 0.7450(3) 0.2377(3) 0.78315(19) 0.0346(6) Uani 1 1 d . . . C9 C 0.7774(4) 0.1711(3) 0.8378(2) 0.0477(7) Uani 1 1 d . . . H9 H 0.8427 0.1180 0.8148 0.057 Uiso 1 1 calc R . . C10 C 0.7142(5) 0.1824(4) 0.9256(3) 0.0660(11) Uani 1 1 d . . . H10 H 0.7375 0.1386 0.9637 0.079 Uiso 1 1 calc R . . C11 C 0.6190(4) 0.2565(4) 0.9566(3) 0.0692(12) Uani 1 1 d . . . H11 H 0.5750 0.2632 1.0165 0.083 Uiso 1 1 calc R . . C12 C 0.5846(4) 0.3217(4) 0.9037(3) 0.0606(10) Uani 1 1 d . . . H12 H 0.5170 0.3726 0.9268 0.073 Uiso 1 1 calc R . . C13 C 0.6486(3) 0.3137(3) 0.8157(2) 0.0435(7) Uani 1 1 d . . . H13 H 0.6262 0.3595 0.7790 0.052 Uiso 1 1 calc R . . C14 C 1.2932(3) 0.4601(3) 0.7553(2) 0.0461(7) Uani 1 1 d . . . H14A H 1.3547 0.4000 0.7319 0.069 Uiso 1 1 calc R . . H14B H 1.3495 0.5394 0.8129 0.069 Uiso 1 1 calc R . . H14C H 1.2649 0.4804 0.6995 0.069 Uiso 1 1 calc R . . C15 C 1.1727(4) 0.3338(3) 0.8947(2) 0.0499(8) Uani 1 1 d . . . H15A H 1.0824 0.3016 0.9194 0.075 Uiso 1 1 calc R . . H15B H 1.2396 0.4073 0.9515 0.075 Uiso 1 1 calc R . . H15C H 1.2222 0.2653 0.8651 0.075 Uiso 1 1 calc R . . C16 C 1.0235(3) 0.5106(3) 0.8551(2) 0.0476(8) Uani 1 1 d . . . H16A H 0.9836 0.5310 0.8025 0.071 Uiso 1 1 calc R . . H16B H 1.0923 0.5885 0.9071 0.071 Uiso 1 1 calc R . . H16C H 0.9418 0.4781 0.8868 0.071 Uiso 1 1 calc R . . O2 O 0.755(2) 0.850(2) 0.7886(18) 0.265(10) Uani 0.619(13) 1 d PDU A 1 C17 C 0.673(3) 0.7243(19) 0.7740(16) 0.191(12) Uani 0.619(13) 1 d PDU A 1 H17A H 0.5656 0.7192 0.7748 0.229 Uiso 0.619(13) 1 calc PR A 1 H17B H 0.6856 0.6593 0.7076 0.229 Uiso 0.619(13) 1 calc PR A 1 C18 C 0.7268(17) 0.7009(18) 0.8547(19) 0.165(11) Uani 0.619(13) 1 d PDU A 1 H18A H 0.7709 0.6275 0.8277 0.198 Uiso 0.619(13) 1 calc PR A 1 H18B H 0.6454 0.6806 0.8927 0.198 Uiso 0.619(13) 1 calc PR A 1 C19 C 0.836(3) 0.8151(18) 0.9193(10) 0.145(8) Uani 0.619(13) 1 d PDU A 1 H19A H 0.8005 0.8555 0.9857 0.174 Uiso 0.619(13) 1 calc PR A 1 H19B H 0.9282 0.7939 0.9318 0.174 Uiso 0.619(13) 1 calc PR A 1 C20 C 0.865(2) 0.9025(18) 0.8739(16) 0.115(7) Uani 0.619(13) 1 d PDU A 1 H20A H 0.8596 0.9888 0.9223 0.137 Uiso 0.619(13) 1 calc PR A 1 H20B H 0.9653 0.9104 0.8522 0.137 Uiso 0.619(13) 1 calc PR A 1 O2A O 0.804(3) 0.8988(14) 0.8733(11) 0.109(7) Uani 0.381(13) 1 d PDU A 2 C17A C 0.7612(19) 0.8030(16) 0.7708(8) 0.081(5) Uani 0.381(13) 1 d PDU A 2 H17C H 0.8502 0.7901 0.7368 0.097 Uiso 0.381(13) 1 calc PR A 2 H17D H 0.6989 0.8301 0.7321 0.097 Uiso 0.381(13) 1 calc PR A 2 C18A C 0.679(3) 0.6858(18) 0.7743(10) 0.094(6) Uani 0.381(13) 1 d PDU A 2 H18C H 0.5760 0.6599 0.7408 0.113 Uiso 0.381(13) 1 calc PR A 2 H18D H 0.7258 0.6158 0.7384 0.113 Uiso 0.381(13) 1 calc PR A 2 C19A C 0.680(2) 0.709(2) 0.8792(12) 0.107(8) Uani 0.381(13) 1 d PDU A 2 H19C H 0.5792 0.7085 0.8990 0.129 Uiso 0.381(13) 1 calc PR A 2 H19D H 0.7118 0.6418 0.8914 0.129 Uiso 0.381(13) 1 calc PR A 2 C20A C 0.781(5) 0.832(2) 0.9368(14) 0.22(2) Uani 0.381(13) 1 d PDU A 2 H20C H 0.7399 0.8811 0.9983 0.259 Uiso 0.381(13) 1 calc PR A 2 H20D H 0.8763 0.8223 0.9586 0.259 Uiso 0.381(13) 1 calc PR A 2 O3 O 0.7183(10) 0.2046(5) 1.1619(5) 0.084(2) Uani 0.619(13) 1 d PDU A 1 C21 C 0.630(2) 0.0778(14) 1.1361(12) 0.099(7) Uani 0.619(13) 1 d PDU A 1 H21A H 0.6711 0.0138 1.0835 0.119 Uiso 0.619(13) 1 calc PR A 1 H21B H 0.5269 0.0665 1.1105 0.119 Uiso 0.619(13) 1 calc PR A 1 C22 C 0.638(2) 0.0652(19) 1.2295(14) 0.256(16) Uani 0.619(13) 1 d PDU A 1 H22A H 0.6295 -0.0256 1.2159 0.307 Uiso 0.619(13) 1 calc PR A 1 H22B H 0.5561 0.0915 1.2670 0.307 Uiso 0.619(13) 1 calc PR A 1 C23 C 0.7774(10) 0.1459(8) 1.2881(7) 0.070(3) Uani 0.619(13) 1 d PDU A 1 H23A H 0.8550 0.0994 1.2724 0.084 Uiso 0.619(13) 1 calc PR A 1 H23B H 0.7705 0.1786 1.3620 0.084 Uiso 0.619(13) 1 calc PR A 1 C24 C 0.8076(11) 0.2488(6) 1.2563(6) 0.079(3) Uani 0.619(13) 1 d PDU A 1 H24A H 0.7838 0.3254 1.3078 0.095 Uiso 0.619(13) 1 calc PR A 1 H24B H 0.9138 0.2730 1.2485 0.095 Uiso 0.619(13) 1 calc PR A 1 O3A O 0.760(3) 0.138(4) 1.1397(16) 0.221(13) Uani 0.381(13) 1 d PDU A 2 C21A C 0.611(2) 0.101(3) 1.1550(14) 0.086(9) Uani 0.381(13) 1 d PDU A 2 H21C H 0.5550 0.0210 1.0961 0.103 Uiso 0.381(13) 1 calc PR A 2 H21D H 0.5621 0.1697 1.1634 0.103 Uiso 0.381(13) 1 calc PR A 2 C22A C 0.6137(12) 0.0803(18) 1.2451(10) 0.066(5) Uani 0.381(13) 1 d PDU A 2 H22C H 0.5273 0.0988 1.2807 0.079 Uiso 0.381(13) 1 calc PR A 2 H22D H 0.6137 -0.0096 1.2291 0.079 Uiso 0.381(13) 1 calc PR A 2 C23A C 0.748(2) 0.168(3) 1.3053(13) 0.22(2) Uani 0.381(13) 1 d PDU A 2 H23C H 0.7325 0.2531 1.3481 0.263 Uiso 0.381(13) 1 calc PR A 2 H23D H 0.7880 0.1353 1.3503 0.263 Uiso 0.381(13) 1 calc PR A 2 C24A C 0.8470(19) 0.179(5) 1.234(2) 0.29(3) Uani 0.381(13) 1 d PDU A 2 H24C H 0.9075 0.2688 1.2580 0.352 Uiso 0.381(13) 1 calc PR A 2 H24D H 0.9145 0.1236 1.2275 0.352 Uiso 0.381(13) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0234(4) 0.0194(4) 0.0286(4) 0.0083(3) 0.0016(3) 0.0036(3) Cl1 0.0369(4) 0.0304(3) 0.0426(4) 0.0213(3) 0.0109(3) 0.0101(3) Cl2 0.0324(3) 0.0398(4) 0.0368(4) 0.0133(3) -0.0024(3) 0.0120(3) N1 0.0255(10) 0.0221(10) 0.0300(11) 0.0084(9) 0.0032(8) 0.0041(8) O1 0.0234(8) 0.0210(8) 0.0336(9) 0.0062(7) 0.0056(7) 0.0038(7) P1 0.0250(3) 0.0206(3) 0.0275(3) 0.0079(3) 0.0048(2) 0.0033(2) Si1 0.0291(4) 0.0280(4) 0.0324(4) 0.0033(3) 0.0013(3) 0.0014(3) C1 0.0248(12) 0.0238(12) 0.0372(14) 0.0076(11) 0.0077(10) 0.0037(10) C2 0.0281(13) 0.0298(13) 0.0344(13) 0.0126(11) 0.0089(10) 0.0114(10) C3 0.0290(13) 0.0434(16) 0.0509(17) 0.0258(14) 0.0131(12) 0.0100(12) C4 0.0315(15) 0.068(2) 0.073(2) 0.0425(19) 0.0126(14) 0.0230(15) C5 0.0448(17) 0.068(2) 0.079(2) 0.052(2) 0.0243(16) 0.0354(16) C6 0.0422(16) 0.0438(17) 0.075(2) 0.0393(17) 0.0260(15) 0.0218(14) C7 0.0314(13) 0.0322(14) 0.0475(15) 0.0189(12) 0.0132(11) 0.0132(11) C8 0.0307(13) 0.0317(14) 0.0293(13) 0.0075(11) 0.0061(10) -0.0032(11) C9 0.0512(18) 0.0466(18) 0.0383(15) 0.0204(14) 0.0033(13) -0.0034(14) C10 0.074(2) 0.066(2) 0.0376(17) 0.0222(17) 0.0010(17) -0.018(2) C11 0.059(2) 0.078(3) 0.0307(16) 0.0066(18) 0.0108(15) -0.022(2) C12 0.0396(17) 0.064(2) 0.0418(18) -0.0043(17) 0.0110(14) -0.0014(15) C13 0.0337(14) 0.0444(17) 0.0342(14) 0.0037(13) 0.0071(11) 0.0019(12) C14 0.0342(15) 0.0301(15) 0.0529(18) 0.0036(13) 0.0050(13) -0.0029(12) C15 0.0438(17) 0.058(2) 0.0344(15) 0.0100(14) -0.0026(12) 0.0089(15) C16 0.0403(16) 0.0333(15) 0.0471(17) -0.0015(13) 0.0060(13) 0.0046(13) O2 0.28(2) 0.26(2) 0.31(2) 0.209(19) -0.044(16) 0.025(15) C17 0.26(3) 0.110(15) 0.177(19) 0.033(12) 0.034(18) 0.048(17) C18 0.125(11) 0.195(18) 0.32(3) 0.21(2) 0.114(16) 0.111(12) C19 0.29(2) 0.126(12) 0.064(7) 0.045(8) 0.012(10) 0.123(15) C20 0.123(12) 0.099(10) 0.115(11) 0.029(8) 0.006(8) 0.049(9) O2A 0.166(19) 0.061(7) 0.090(9) 0.023(6) -0.025(11) 0.035(9) C17A 0.092(10) 0.120(14) 0.039(6) 0.052(7) 0.019(6) 0.011(8) C18A 0.156(18) 0.071(11) 0.058(8) 0.035(7) 0.036(9) 0.020(10) C19A 0.140(18) 0.158(19) 0.073(10) 0.080(12) 0.062(11) 0.067(15) C20A 0.40(6) 0.15(3) 0.095(17) 0.033(17) 0.09(3) 0.10(4) O3 0.139(6) 0.052(3) 0.057(3) 0.034(2) -0.004(3) -0.001(3) C21 0.130(13) 0.076(8) 0.068(6) 0.033(6) -0.011(7) -0.017(8) C22 0.22(2) 0.22(2) 0.35(3) 0.24(2) -0.149(19) -0.118(16) C23 0.072(5) 0.065(5) 0.075(6) 0.045(5) -0.021(4) -0.001(4) C24 0.099(7) 0.052(4) 0.079(5) 0.037(4) -0.006(4) -0.007(4) O3A 0.25(3) 0.29(3) 0.132(15) 0.15(2) 0.047(16) 0.01(2) C21A 0.096(14) 0.094(17) 0.068(12) 0.031(10) -0.003(9) 0.035(13) C22A 0.045(6) 0.115(13) 0.058(7) 0.054(8) 0.004(6) 0.028(8) C23A 0.40(5) 0.107(18) 0.103(16) -0.003(13) 0.13(3) 0.06(2) C24A 0.052(11) 0.61(7) 0.28(4) 0.30(5) -0.013(16) 0.00(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.8269(17) . ? Al1 O1 1.9205(18) 2_756 ? Al1 N1 1.969(2) . ? Al1 Cl2 2.1698(9) . ? Al1 Cl1 2.1720(9) . ? N1 P1 1.601(2) . ? N1 Si1 1.764(2) . ? O1 C1 1.411(3) . ? O1 Al1 1.9205(18) 2_756 ? P1 C8 1.792(3) . ? P1 C2 1.794(3) . ? P1 C1 1.821(3) . ? Si1 C15 1.853(3) . ? Si1 C14 1.856(3) . ? Si1 C16 1.865(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C7 1.387(4) . ? C2 C3 1.390(4) . ? C3 C4 1.382(4) . ? C3 H3 0.9500 . ? C4 C5 1.376(5) . ? C4 H4 0.9500 . ? C5 C6 1.379(5) . ? C5 H5 0.9500 . ? C6 C7 1.385(4) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C13 1.382(4) . ? C8 C9 1.397(4) . ? C9 C10 1.384(5) . ? C9 H9 0.9500 . ? C10 C11 1.356(6) . ? C10 H10 0.9500 . ? C11 C12 1.371(6) . ? C11 H11 0.9500 . ? C12 C13 1.399(4) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? O2 C20 1.413(8) . ? O2 C17 1.426(8) . ? C17 C18 1.417(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.417(8) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.414(8) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? O2A C20A 1.423(9) . ? O2A C17A 1.427(8) . ? C17A C18A 1.434(9) . ? C17A H17C 0.9900 . ? C17A H17D 0.9900 . ? C18A C19A 1.430(8) . ? C18A H18C 0.9900 . ? C18A H18D 0.9900 . ? C19A C20A 1.424(9) . ? C19A H19C 0.9900 . ? C19A H19D 0.9900 . ? C20A H20C 0.9900 . ? C20A H20D 0.9900 . ? O3 C21 1.414(8) . ? O3 C24 1.416(6) . ? C21 C22 1.422(8) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.424(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.436(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? O3A C24A 1.416(9) . ? O3A C21A 1.416(9) . ? C21A C22A 1.424(9) . ? C21A H21C 0.9900 . ? C21A H21D 0.9900 . ? C22A C23A 1.420(9) . ? C22A H22C 0.9900 . ? C22A H22D 0.9900 . ? C23A C24A 1.420(9) . ? C23A H23C 0.9900 . ? C23A H23D 0.9900 . ? C24A H24C 0.9900 . ? C24A H24D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 O1 72.92(8) . 2_756 ? O1 Al1 N1 88.25(8) . . ? O1 Al1 N1 160.34(9) 2_756 . ? O1 Al1 Cl2 130.77(7) . . ? O1 Al1 Cl2 90.99(6) 2_756 . ? N1 Al1 Cl2 97.35(7) . . ? O1 Al1 Cl1 114.95(7) . . ? O1 Al1 Cl1 92.90(6) 2_756 . ? N1 Al1 Cl1 100.35(7) . . ? Cl2 Al1 Cl1 112.00(4) . . ? P1 N1 Si1 123.18(12) . . ? P1 N1 Al1 111.91(11) . . ? Si1 N1 Al1 124.85(11) . . ? C1 O1 Al1 124.57(15) . . ? C1 O1 Al1 127.95(14) . 2_756 ? Al1 O1 Al1 107.08(8) . 2_756 ? N1 P1 C8 115.74(12) . . ? N1 P1 C2 113.96(12) . . ? C8 P1 C2 108.82(13) . . ? N1 P1 C1 103.51(11) . . ? C8 P1 C1 106.30(12) . . ? C2 P1 C1 107.83(12) . . ? N1 Si1 C15 110.28(13) . . ? N1 Si1 C14 109.60(12) . . ? C15 Si1 C14 110.76(15) . . ? N1 Si1 C16 111.07(12) . . ? C15 Si1 C16 107.47(16) . . ? C14 Si1 C16 107.61(14) . . ? O1 C1 P1 105.08(15) . . ? O1 C1 H1A 110.7 . . ? P1 C1 H1A 110.7 . . ? O1 C1 H1B 110.7 . . ? P1 C1 H1B 110.7 . . ? H1A C1 H1B 108.8 . . ? C7 C2 C3 119.5(2) . . ? C7 C2 P1 119.3(2) . . ? C3 C2 P1 121.2(2) . . ? C4 C3 C2 120.1(3) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C5 C4 C3 120.1(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.3(3) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C7 120.0(3) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C6 C7 C2 120.0(3) . . ? C6 C7 H7 120.0 . . ? C2 C7 H7 120.0 . . ? C13 C8 C9 120.2(3) . . ? C13 C8 P1 123.2(2) . . ? C9 C8 P1 116.6(2) . . ? C10 C9 C8 120.0(4) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C10 C9 119.5(4) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 121.5(3) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C11 C12 C13 120.2(4) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C8 C13 C12 118.6(3) . . ? C8 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C20 O2 C17 109.4(11) . . ? C18 C17 O2 107.4(10) . . ? C18 C17 H17A 110.2 . . ? O2 C17 H17A 110.2 . . ? C18 C17 H17B 110.2 . . ? O2 C17 H17B 110.2 . . ? H17A C17 H17B 108.5 . . ? C17 C18 C19 106.6(10) . . ? C17 C18 H18A 110.4 . . ? C19 C18 H18A 110.4 . . ? C17 C18 H18B 110.4 . . ? C19 C18 H18B 110.4 . . ? H18A C18 H18B 108.6 . . ? C20 C19 C18 110.2(10) . . ? C20 C19 H19A 109.6 . . ? C18 C19 H19A 109.6 . . ? C20 C19 H19B 109.6 . . ? C18 C19 H19B 109.6 . . ? H19A C19 H19B 108.1 . . ? O2 C20 C19 105.4(10) . . ? O2 C20 H20A 110.7 . . ? C19 C20 H20A 110.6 . . ? O2 C20 H20B 110.7 . . ? C19 C20 H20B 110.7 . . ? H20A C20 H20B 108.8 . . ? C20A O2A C17A 106.5(10) . . ? O2A C17A C18A 107.6(9) . . ? O2A C17A H17C 110.2 . . ? C18A C17A H17C 110.2 . . ? O2A C17A H17D 110.2 . . ? C18A C17A H17D 110.2 . . ? H17C C17A H17D 108.5 . . ? C19A C18A C17A 107.6(10) . . ? C19A C18A H18C 110.2 . . ? C17A C18A H18C 110.2 . . ? C19A C18A H18D 110.2 . . ? C17A C18A H18D 110.2 . . ? H18C C18A H18D 108.5 . . ? C20A C19A C18A 106.7(11) . . ? C20A C19A H19C 110.4 . . ? C18A C19A H19C 110.4 . . ? C20A C19A H19D 110.4 . . ? C18A C19A H19D 110.4 . . ? H19C C19A H19D 108.6 . . ? O2A C20A C19A 107.7(13) . . ? O2A C20A H20C 110.2 . . ? C19A C20A H20C 110.2 . . ? O2A C20A H20D 110.1 . . ? C19A C20A H20D 110.1 . . ? H20C C20A H20D 108.5 . . ? C21 O3 C24 108.4(6) . . ? O3 C21 C22 103.8(8) . . ? O3 C21 H21A 111.0 . . ? C22 C21 H21A 111.0 . . ? O3 C21 H21B 111.0 . . ? C22 C21 H21B 111.0 . . ? H21A C21 H21B 109.0 . . ? C21 C22 C23 107.7(9) . . ? C21 C22 H22A 110.1 . . ? C23 C22 H22A 110.1 . . ? C21 C22 H22B 110.2 . . ? C23 C22 H22B 110.2 . . ? H22A C22 H22B 108.5 . . ? C22 C23 C24 102.9(7) . . ? C22 C23 H23A 111.2 . . ? C24 C23 H23A 111.2 . . ? C22 C23 H23B 111.2 . . ? C24 C23 H23B 111.2 . . ? H23A C23 H23B 109.1 . . ? O3 C24 C23 107.7(5) . . ? O3 C24 H24A 110.2 . . ? C23 C24 H24A 110.2 . . ? O3 C24 H24B 110.2 . . ? C23 C24 H24B 110.2 . . ? H24A C24 H24B 108.5 . . ? C24A O3A C21A 106.2(10) . . ? O3A C21A C22A 106.4(10) . . ? O3A C21A H21C 110.5 . . ? C22A C21A H21C 110.4 . . ? O3A C21A H21D 110.4 . . ? C22A C21A H21D 110.5 . . ? H21C C21A H21D 108.6 . . ? C23A C22A C21A 104.0(12) . . ? C23A C22A H22C 110.9 . . ? C21A C22A H22C 111.0 . . ? C23A C22A H22D 111.0 . . ? C21A C22A H22D 111.0 . . ? H22C C22A H22D 109.0 . . ? C24A C23A C22A 105.3(12) . . ? C24A C23A H23C 110.7 . . ? C22A C23A H23C 110.7 . . ? C24A C23A H23D 110.7 . . ? C22A C23A H23D 110.7 . . ? H23C C23A H23D 108.8 . . ? O3A C24A C23A 107.6(11) . . ? O3A C24A H24C 110.2 . . ? C23A C24A H24C 110.2 . . ? O3A C24A H24D 110.2 . . ? C23A C24A H24D 110.2 . . ? H24C C24A H24D 108.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Al1 N1 P1 -16.61(12) . . . . ? O1 Al1 N1 P1 -33.1(3) 2_756 . . . ? Cl2 Al1 N1 P1 -147.52(10) . . . . ? Cl1 Al1 N1 P1 98.44(11) . . . . ? O1 Al1 N1 Si1 166.18(14) . . . . ? O1 Al1 N1 Si1 149.6(2) 2_756 . . . ? Cl2 Al1 N1 Si1 35.27(14) . . . . ? Cl1 Al1 N1 Si1 -78.77(13) . . . . ? O1 Al1 O1 C1 173.2(2) 2_756 . . . ? N1 Al1 O1 C1 -1.0(2) . . . . ? Cl2 Al1 O1 C1 97.17(19) . . . . ? Cl1 Al1 O1 C1 -101.63(19) . . . . ? O1 Al1 O1 Al1 0.0 2_756 . . 2_756 ? N1 Al1 O1 Al1 -174.25(10) . . . 2_756 ? Cl2 Al1 O1 Al1 -76.05(10) . . . 2_756 ? Cl1 Al1 O1 Al1 85.15(9) . . . 2_756 ? Si1 N1 P1 C8 -41.43(19) . . . . ? Al1 N1 P1 C8 141.30(13) . . . . ? Si1 N1 P1 C2 85.88(17) . . . . ? Al1 N1 P1 C2 -91.38(14) . . . . ? Si1 N1 P1 C1 -157.29(15) . . . . ? Al1 N1 P1 C1 25.44(15) . . . . ? P1 N1 Si1 C15 97.61(18) . . . . ? Al1 N1 Si1 C15 -85.48(17) . . . . ? P1 N1 Si1 C14 -140.20(17) . . . . ? Al1 N1 Si1 C14 36.70(19) . . . . ? P1 N1 Si1 C16 -21.4(2) . . . . ? Al1 N1 Si1 C16 155.48(16) . . . . ? Al1 O1 C1 P1 15.5(2) . . . . ? Al1 O1 C1 P1 -172.72(11) 2_756 . . . ? N1 P1 C1 O1 -24.80(19) . . . . ? C8 P1 C1 O1 -147.19(17) . . . . ? C2 P1 C1 O1 96.26(18) . . . . ? N1 P1 C2 C7 -8.8(3) . . . . ? C8 P1 C2 C7 122.0(2) . . . . ? C1 P1 C2 C7 -123.1(2) . . . . ? N1 P1 C2 C3 170.0(2) . . . . ? C8 P1 C2 C3 -59.2(2) . . . . ? C1 P1 C2 C3 55.7(2) . . . . ? C7 C2 C3 C4 -0.7(4) . . . . ? P1 C2 C3 C4 -179.5(2) . . . . ? C2 C3 C4 C5 0.0(5) . . . . ? C3 C4 C5 C6 0.3(5) . . . . ? C4 C5 C6 C7 0.1(5) . . . . ? C5 C6 C7 C2 -0.8(5) . . . . ? C3 C2 C7 C6 1.1(4) . . . . ? P1 C2 C7 C6 179.9(2) . . . . ? N1 P1 C8 C13 125.1(2) . . . . ? C2 P1 C8 C13 -4.7(3) . . . . ? C1 P1 C8 C13 -120.6(2) . . . . ? N1 P1 C8 C9 -54.5(2) . . . . ? C2 P1 C8 C9 175.6(2) . . . . ? C1 P1 C8 C9 59.8(2) . . . . ? C13 C8 C9 C10 -0.9(4) . . . . ? P1 C8 C9 C10 178.8(2) . . . . ? C8 C9 C10 C11 1.3(5) . . . . ? C9 C10 C11 C12 -0.7(5) . . . . ? C10 C11 C12 C13 -0.4(5) . . . . ? C9 C8 C13 C12 -0.2(4) . . . . ? P1 C8 C13 C12 -179.8(2) . . . . ? C11 C12 C13 C8 0.8(4) . . . . ? C20 O2 C17 C18 3(3) . . . . ? O2 C17 C18 C19 3(3) . . . . ? C17 C18 C19 C20 -8(3) . . . . ? C17 O2 C20 C19 -8(3) . . . . ? C18 C19 C20 O2 10(3) . . . . ? C20A O2A C17A C18A 14(3) . . . . ? O2A C17A C18A C19A -3(3) . . . . ? C17A C18A C19A C20A -9(3) . . . . ? C17A O2A C20A C19A -20(4) . . . . ? C18A C19A C20A O2A 18(4) . . . . ? C24 O3 C21 C22 17(2) . . . . ? O3 C21 C22 C23 -30(2) . . . . ? C21 C22 C23 C24 30(2) . . . . ? C21 O3 C24 C23 1.6(15) . . . . ? C22 C23 C24 O3 -19.2(16) . . . . ? C24A O3A C21A C22A -19(4) . . . . ? O3A C21A C22A C23A 31(3) . . . . ? C21A C22A C23A C24A -32(4) . . . . ? C21A O3A C24A C23A -1(5) . . . . ? C22A C23A C24A O3A 21(5) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.443 _refine_diff_density_min -0.239 _refine_diff_density_rms 0.063 #===END data_complex_8 _database_code_depnum_ccdc_archive 'CCDC 775395' #TrackingRef 'cif_complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H32 Al2 Cl4 N2 O P2' _chemical_formula_weight 694.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4330(15) _cell_length_b 9.7126(17) _cell_length_c 11.539(2) _cell_angle_alpha 91.184(3) _cell_angle_beta 94.033(3) _cell_angle_gamma 111.992(3) _cell_volume 873.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 358 _exptl_absorpt_coefficient_mu 0.507 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8966 _exptl_absorpt_correction_T_max 0.9417 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8486 _diffrn_reflns_av_R_equivalents 0.1161 _diffrn_reflns_av_sigmaI/netI 0.0866 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3059 _reflns_number_gt 2634 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0735P)^2^+0.0418P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3059 _refine_ls_number_parameters 186 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0470 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1254 _refine_ls_wR_factor_gt 0.1213 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.968 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.44765(8) 0.55226(8) 0.40554(5) 0.0203(2) Uani 1 1 d . . . N1 N 0.4726(2) 0.5981(2) 0.56411(15) 0.0217(5) Uani 1 1 d . . . P1 P 0.44759(7) 0.72369(7) 0.64189(5) 0.0203(2) Uani 1 1 d . . . Cl1 Cl 0.18981(7) 0.47569(7) 0.32869(5) 0.0340(2) Uani 1 1 d . . . Cl2 Cl 0.60217(8) 0.73069(7) 0.30833(5) 0.0309(2) Uani 1 1 d . . . C1 C 0.2823(3) 0.7788(3) 0.5768(2) 0.0299(6) Uani 1 1 d . . . H1B H 0.1724 0.6939 0.5712 0.045 Uiso 1 1 calc R . . H1C H 0.3105 0.8129 0.4987 0.045 Uiso 1 1 calc R . . H1D H 0.2737 0.8598 0.6248 0.045 Uiso 1 1 calc R . . C2 C 0.3890(3) 0.6609(3) 0.78368(19) 0.0221(5) Uani 1 1 d . . . C3 C 0.5037(3) 0.7123(3) 0.8831(2) 0.0350(7) Uani 1 1 d . . . H3A H 0.6163 0.7831 0.8771 0.042 Uiso 1 1 calc R . . C4 C 0.4521(4) 0.6594(3) 0.9901(2) 0.0443(8) Uani 1 1 d . . . H4A H 0.5299 0.6937 1.0577 0.053 Uiso 1 1 calc R . . C5 C 0.2888(4) 0.5573(3) 0.9993(2) 0.0441(8) Uani 1 1 d . . . H5A H 0.2538 0.5232 1.0734 0.053 Uiso 1 1 calc R . . C6 C 0.1760(4) 0.5044(3) 0.9021(2) 0.0396(7) Uani 1 1 d . . . H6A H 0.0642 0.4325 0.9088 0.048 Uiso 1 1 calc R . . C7 C 0.2253(3) 0.5561(3) 0.7943(2) 0.0308(6) Uani 1 1 d . . . H7A H 0.1470 0.5198 0.7272 0.037 Uiso 1 1 calc R . . C8 C 0.6370(3) 0.8918(3) 0.66501(19) 0.0245(5) Uani 1 1 d . . . C9 C 0.7903(3) 0.8990(3) 0.6230(2) 0.0293(6) Uani 1 1 d . . . H9A H 0.7951 0.8164 0.5799 0.035 Uiso 1 1 calc R . . C10 C 0.9359(3) 1.0271(3) 0.6442(2) 0.0356(7) Uani 1 1 d . . . H10A H 1.0411 1.0319 0.6163 0.043 Uiso 1 1 calc R . . C11 C 0.9292(3) 1.1476(3) 0.7057(2) 0.0383(7) Uani 1 1 d . . . H11A H 1.0299 1.2348 0.7203 0.046 Uiso 1 1 calc R . . C12 C 0.7773(3) 1.1421(3) 0.7460(2) 0.0356(6) Uani 1 1 d . . . H12A H 0.7728 1.2259 0.7876 0.043 Uiso 1 1 calc R . . C13 C 0.6312(3) 1.0146(3) 0.7258(2) 0.0304(6) Uani 1 1 d . . . H13A H 0.5263 1.0109 0.7536 0.037 Uiso 1 1 calc R . . O1 O 0.9406(4) 0.9655(4) 0.9830(3) 0.0434(10) Uiso 0.50 1 d PD . . C14 C 1.0552(8) 0.9029(8) 0.9542(6) 0.0529(17) Uiso 0.50 1 d PD . 1 C15 C 1.2220(9) 0.9376(9) 0.9123(7) 0.066(2) Uiso 0.50 1 d PD A 1 H15A H 1.2197 0.8556 0.8604 0.099 Uiso 0.50 1 calc PR A 1 H15B H 1.3073 0.9521 0.9783 0.099 Uiso 0.50 1 calc PR A 1 H15C H 1.2526 1.0289 0.8695 0.099 Uiso 0.50 1 calc PR A 1 C14A C 1.1027(8) 0.9831(8) 0.9459(6) 0.0516(17) Uiso 0.50 1 d PD . 2 C15A C 1.0942(10) 0.8506(8) 0.8857(6) 0.0630(19) Uiso 0.50 1 d PD B 2 H15D H 1.2105 0.8576 0.8725 0.094 Uiso 0.50 1 calc PR B 2 H15E H 1.0269 0.8381 0.8107 0.094 Uiso 0.50 1 calc PR B 2 H15F H 1.0393 0.7650 0.9323 0.094 Uiso 0.50 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0192(4) 0.0242(4) 0.0159(4) -0.0022(3) -0.0013(3) 0.0070(3) N1 0.0200(10) 0.0245(11) 0.0179(10) -0.0019(8) -0.0007(7) 0.0057(8) P1 0.0192(3) 0.0241(4) 0.0168(3) -0.0017(3) 0.0001(2) 0.0075(3) Cl1 0.0232(3) 0.0391(4) 0.0345(4) -0.0004(3) -0.0091(3) 0.0080(3) Cl2 0.0298(4) 0.0329(4) 0.0267(4) 0.0061(3) 0.0039(2) 0.0076(3) C1 0.0318(14) 0.0370(16) 0.0252(13) 0.0001(11) -0.0020(10) 0.0187(12) C2 0.0273(12) 0.0236(13) 0.0178(11) -0.0019(9) 0.0031(9) 0.0123(10) C3 0.0348(14) 0.0395(17) 0.0250(14) -0.0004(12) -0.0024(11) 0.0086(12) C4 0.061(2) 0.0500(19) 0.0183(13) -0.0003(12) -0.0031(12) 0.0186(16) C5 0.064(2) 0.0469(19) 0.0264(15) 0.0095(13) 0.0195(14) 0.0239(16) C6 0.0390(16) 0.0387(17) 0.0378(16) 0.0053(13) 0.0155(13) 0.0084(13) C7 0.0273(13) 0.0344(15) 0.0289(14) -0.0013(11) 0.0046(10) 0.0093(12) C8 0.0255(12) 0.0250(14) 0.0204(12) -0.0006(10) -0.0024(10) 0.0074(11) C9 0.0297(13) 0.0276(15) 0.0284(13) -0.0049(11) 0.0025(10) 0.0088(11) C10 0.0247(13) 0.0351(16) 0.0416(16) -0.0021(13) 0.0037(11) 0.0053(12) C11 0.0310(14) 0.0295(16) 0.0432(16) -0.0026(12) -0.0029(12) -0.0001(12) C12 0.0413(16) 0.0240(15) 0.0371(15) -0.0056(12) -0.0007(12) 0.0082(12) C13 0.0338(14) 0.0291(15) 0.0294(13) 0.0001(11) 0.0033(11) 0.0129(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 N1 1.852(2) 2_666 ? Al1 N1 1.8526(19) . ? Al1 Cl2 2.1340(10) . ? Al1 Cl1 2.1349(9) . ? Al1 Al1 2.6560(14) 2_666 ? N1 P1 1.5853(19) . ? N1 Al1 1.852(2) 2_666 ? P1 C1 1.795(2) . ? P1 C2 1.795(2) . ? P1 C8 1.805(2) . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C2 C7 1.390(3) . ? C2 C3 1.400(3) . ? C3 C4 1.383(4) . ? C3 H3A 0.9500 . ? C4 C5 1.376(4) . ? C4 H4A 0.9500 . ? C5 C6 1.374(4) . ? C5 H5A 0.9500 . ? C6 C7 1.383(4) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.391(3) . ? C8 C13 1.390(3) . ? C9 C10 1.384(3) . ? C9 H9A 0.9500 . ? C10 C11 1.377(4) . ? C10 H10A 0.9500 . ? C11 C12 1.377(4) . ? C11 H11A 0.9500 . ? C12 C13 1.382(4) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? O1 O1 1.018(7) 2_777 ? O1 C14A 1.104(7) 2_777 ? O1 C14 1.375(6) . ? O1 C14A 1.411(6) . ? O1 C14 1.444(8) 2_777 ? C14 C15 1.440(6) . ? C14 O1 1.444(8) 2_777 ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C14A O1 1.104(7) 2_777 ? C14A C15A 1.425(6) . ? C15A H15D 0.9800 . ? C15A H15E 0.9800 . ? C15A H15F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Al1 N1 88.39(9) 2_666 . ? N1 Al1 Cl2 117.03(7) 2_666 . ? N1 Al1 Cl2 113.35(7) . . ? N1 Al1 Cl1 114.10(7) 2_666 . ? N1 Al1 Cl1 114.83(7) . . ? Cl2 Al1 Cl1 108.28(4) . . ? N1 Al1 Al1 44.21(6) 2_666 2_666 ? N1 Al1 Al1 44.18(7) . 2_666 ? Cl2 Al1 Al1 126.40(4) . 2_666 ? Cl1 Al1 Al1 125.29(5) . 2_666 ? P1 N1 Al1 134.30(11) . 2_666 ? P1 N1 Al1 133.97(13) . . ? Al1 N1 Al1 91.61(9) 2_666 . ? N1 P1 C1 111.39(11) . . ? N1 P1 C2 111.26(11) . . ? C1 P1 C2 107.69(11) . . ? N1 P1 C8 113.93(11) . . ? C1 P1 C8 105.89(12) . . ? C2 P1 C8 106.29(11) . . ? P1 C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? C7 C2 C3 119.2(2) . . ? C7 C2 P1 118.73(18) . . ? C3 C2 P1 122.06(19) . . ? C4 C3 C2 119.7(3) . . ? C4 C3 H3A 120.2 . . ? C2 C3 H3A 120.2 . . ? C5 C4 C3 120.4(3) . . ? C5 C4 H4A 119.8 . . ? C3 C4 H4A 119.8 . . ? C6 C5 C4 120.5(3) . . ? C6 C5 H5A 119.8 . . ? C4 C5 H5A 119.8 . . ? C5 C6 C7 119.9(3) . . ? C5 C6 H6A 120.0 . . ? C7 C6 H6A 120.0 . . ? C6 C7 C2 120.4(2) . . ? C6 C7 H7A 119.8 . . ? C2 C7 H7A 119.8 . . ? C9 C8 C13 119.5(2) . . ? C9 C8 P1 120.21(19) . . ? C13 C8 P1 120.29(19) . . ? C10 C9 C8 119.6(2) . . ? C10 C9 H9A 120.2 . . ? C8 C9 H9A 120.2 . . ? C11 C10 C9 120.4(2) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C10 C11 C12 120.3(2) . . ? C10 C11 H11A 119.9 . . ? C12 C11 H11A 119.9 . . ? C11 C12 C13 119.9(3) . . ? C11 C12 H12A 120.1 . . ? C13 C12 H12A 120.1 . . ? C12 C13 C8 120.3(2) . . ? C12 C13 H13A 119.9 . . ? C8 C13 H13A 119.9 . . ? O1 O1 C14A 83.3(5) 2_777 2_777 ? O1 O1 C14 72.5(5) 2_777 . ? C14A O1 C14 145.0(6) 2_777 . ? O1 O1 C14A 51.0(4) 2_777 . ? C14A O1 C14A 134.2(4) 2_777 . ? C14 O1 C14A 30.9(4) . . ? O1 O1 C14 65.3(4) 2_777 2_777 ? C14A O1 C14 30.3(5) 2_777 2_777 ? C14 O1 C14 137.7(3) . 2_777 ? C14A O1 C14 111.9(4) . 2_777 ? O1 C14 C15 142.7(7) . . ? O1 C14 O1 42.3(3) . 2_777 ? C15 C14 O1 107.1(6) . 2_777 ? O1 C14A O1 45.8(4) 2_777 . ? O1 C14A C15A 148.0(8) 2_777 . ? O1 C14A C15A 110.3(6) . . ? C14A C15A H15D 109.5 . . ? C14A C15A H15E 109.5 . . ? H15D C15A H15E 109.5 . . ? C14A C15A H15F 109.5 . . ? H15D C15A H15F 109.5 . . ? H15E C15A H15F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Al1 N1 P1 176.3(2) 2_666 . . . ? Cl2 Al1 N1 P1 57.45(17) . . . . ? Cl1 Al1 N1 P1 -67.75(17) . . . . ? Al1 Al1 N1 P1 176.3(2) 2_666 . . . ? N1 Al1 N1 Al1 0.0 2_666 . . 2_666 ? Cl2 Al1 N1 Al1 -118.89(7) . . . 2_666 ? Cl1 Al1 N1 Al1 115.92(7) . . . 2_666 ? Al1 N1 P1 C1 -153.87(16) 2_666 . . . ? Al1 N1 P1 C1 31.3(2) . . . . ? Al1 N1 P1 C2 -33.70(19) 2_666 . . . ? Al1 N1 P1 C2 151.43(15) . . . . ? Al1 N1 P1 C8 86.42(18) 2_666 . . . ? Al1 N1 P1 C8 -88.45(17) . . . . ? N1 P1 C2 C7 -71.5(2) . . . . ? C1 P1 C2 C7 50.8(2) . . . . ? C8 P1 C2 C7 163.9(2) . . . . ? N1 P1 C2 C3 107.3(2) . . . . ? C1 P1 C2 C3 -130.3(2) . . . . ? C8 P1 C2 C3 -17.2(2) . . . . ? C7 C2 C3 C4 -0.7(4) . . . . ? P1 C2 C3 C4 -179.6(2) . . . . ? C2 C3 C4 C5 -0.3(5) . . . . ? C3 C4 C5 C6 1.3(5) . . . . ? C4 C5 C6 C7 -1.3(5) . . . . ? C5 C6 C7 C2 0.3(4) . . . . ? C3 C2 C7 C6 0.7(4) . . . . ? P1 C2 C7 C6 179.6(2) . . . . ? N1 P1 C8 C9 -4.4(2) . . . . ? C1 P1 C8 C9 -127.1(2) . . . . ? C2 P1 C8 C9 118.5(2) . . . . ? N1 P1 C8 C13 176.22(18) . . . . ? C1 P1 C8 C13 53.4(2) . . . . ? C2 P1 C8 C13 -60.9(2) . . . . ? C13 C8 C9 C10 1.3(4) . . . . ? P1 C8 C9 C10 -178.1(2) . . . . ? C8 C9 C10 C11 -0.6(4) . . . . ? C9 C10 C11 C12 -0.4(4) . . . . ? C10 C11 C12 C13 0.7(4) . . . . ? C11 C12 C13 C8 0.0(4) . . . . ? C9 C8 C13 C12 -1.0(4) . . . . ? P1 C8 C13 C12 178.4(2) . . . . ? O1 O1 C14 C15 -43.7(11) 2_777 . . . ? C14A O1 C14 C15 -91.9(15) 2_777 . . . ? C14A O1 C14 C15 -3.1(8) . . . . ? C14 O1 C14 C15 -43.7(11) 2_777 . . . ? C14A O1 C14 O1 -48.2(9) 2_777 . . 2_777 ? C14A O1 C14 O1 40.6(9) . . . 2_777 ? C14 O1 C14 O1 0.000(1) 2_777 . . 2_777 ? C14A O1 C14A O1 0.000(2) 2_777 . . 2_777 ? C14 O1 C14A O1 -126.9(11) . . . 2_777 ? C14 O1 C14A O1 24.9(6) 2_777 . . 2_777 ? O1 O1 C14A C15A 154.4(9) 2_777 . . . ? C14A O1 C14A C15A 154.4(9) 2_777 . . . ? C14 O1 C14A C15A 27.5(7) . . . . ? C14 O1 C14A C15A 179.3(5) 2_777 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.556 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.072 #===END