Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Martin Schroder' 'Andrew J. Atkins' 'Daniel Black' 'Alexander J. Blake' 'Rachel L. Finn' 'Wan-Sheung Li' 'Armando Marin-Becerra' 'L. Ruiz-Ramirez' _publ_contact_author_name 'Prof Martin Schroder' _publ_contact_author_address ; Department of Chemistry The University of Nottingham University Park Nottingham NG7 2RD UNITED KINGDOM ; _publ_contact_author_email M.SCHRODER@NOTTINGHAM.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis and Structure of Mononuclear and Binuclear Zinc(II) Compartmental Macrocyclic Complexes ; data_1 _database_code_CSD 197068 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C26 H28 N4 O6 Zn2, 2(C H Cl3)' _chemical_formula_sum 'C28 H30 Cl6 N4 O6 Zn2' _chemical_formula_weight 862.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.761(2) _cell_length_b 11.358(2) _cell_length_c 11.211(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.233(15) _cell_angle_gamma 90.00 _cell_volume 1738.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 37 _cell_measurement_theta_min 13.5 _cell_measurement_theta_max 17 _exptl_crystal_description Tablet _exptl_crystal_colour Orange _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 1.887 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.329 _exptl_absorpt_correction_T_max 0.448 _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 'Stoe Stadi-4 four-circle' _diffrn_measurement_method Omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 'variation +-3.6' _diffrn_reflns_number 3067 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_sigmaI/netI 0.0172 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3067 _reflns_number_gt 2736 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stadi-4 (Stoe & Cie, 1995a)' _computing_cell_refinement Stadi-4 _computing_data_reduction 'X-Red (Stoe & Cie, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2002)' _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^)+(0.045P)^2^+5.967P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens 'methyl H atoms from circular difference Fourier; others placed geometrically' _refine_ls_hydrogen_treatment 'rigid rotating group; riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3067 _refine_ls_number_parameters 210 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.111 _refine_ls_wR_factor_gt 0.103 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.003 _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 0.08306(3) 0.40726(3) 0.04590(4) 0.02295(15) Uani 1 1 d . . . N1 N 0.0232(2) 0.2450(3) 0.0738(3) 0.0246(6) Uani 1 1 d . . . N2 N 0.1406(2) 0.3186(3) -0.0877(3) 0.0251(7) Uani 1 1 d . . . O1 O -0.04532(19) 0.4713(2) 0.0852(2) 0.0324(6) Uani 1 1 d . . . O2 O 0.1740(2) 0.4897(3) 0.1654(3) 0.0387(7) Uani 1 1 d . . . O3 O 0.2720(2) 0.3368(2) 0.1557(2) 0.0330(6) Uani 1 1 d . . . C1 C -0.1005(3) 0.4331(3) 0.1637(3) 0.0243(8) Uani 1 1 d . . . C2 C -0.0982(3) 0.3126(3) 0.1997(3) 0.0255(8) Uani 1 1 d . . . C3 C -0.1572(3) 0.2765(4) 0.2849(3) 0.0294(8) Uani 1 1 d . . . H3 H -0.1557 0.1960 0.3081 0.035 Uiso 1 1 calc R . . C4 C -0.2179(3) 0.3520(4) 0.3373(3) 0.0318(9) Uani 1 1 d . . . C5 C -0.2216(3) 0.4692(4) 0.2995(3) 0.0286(8) Uani 1 1 d . . . H5 H -0.2635 0.5221 0.3342 0.034 Uiso 1 1 calc R . . C6 C -0.1661(3) 0.5116(3) 0.2129(3) 0.0261(8) Uani 1 1 d . . . C7 C -0.2804(3) 0.3104(5) 0.4312(4) 0.0442(11) Uani 1 1 d . . . H7A H -0.3494 0.3091 0.3963 0.066 Uiso 1 1 calc R . . H7B H -0.2722 0.3642 0.5000 0.066 Uiso 1 1 calc R . . H7C H -0.2600 0.2310 0.4578 0.066 Uiso 1 1 calc R . . C8 C -0.0441(3) 0.2240(3) 0.1397(3) 0.0260(8) Uani 1 1 d . . . H8 H -0.0605 0.1439 0.1507 0.031 Uiso 1 1 calc R . . C9 C 0.0591(3) 0.1528(3) -0.0025(3) 0.0290(8) Uani 1 1 d . . . H9A H 0.0068 0.1326 -0.0683 0.035 Uiso 1 1 calc R . . H9B H 0.0749 0.0810 0.0461 0.035 Uiso 1 1 calc R . . C10 C 0.1507(3) 0.1940(3) -0.0564(4) 0.0292(8) Uani 1 1 d . . . H10A H 0.2096 0.1820 0.0027 0.035 Uiso 1 1 calc R . . H10B H 0.1584 0.1472 -0.1291 0.035 Uiso 1 1 calc R . . C11 C 0.1740(3) 0.3630(3) -0.1798(3) 0.0256(8) Uani 1 1 d . . . H11 H 0.2058 0.3119 -0.2296 0.031 Uiso 1 1 calc R . . C12 C 0.2570(3) 0.4385(4) 0.1873(3) 0.0293(8) Uani 1 1 d . . . C13 C 0.3389(3) 0.5084(4) 0.2570(5) 0.0463(11) Uani 1 1 d . . . H13A H 0.3783 0.5459 0.2007 0.069 Uiso 1 1 calc R . . H13B H 0.3804 0.4556 0.3105 0.069 Uiso 1 1 calc R . . H13C H 0.3110 0.5690 0.3048 0.069 Uiso 1 1 calc R . . C1S C 0.5415(3) 0.7181(4) -0.0526(4) 0.0400(10) Uani 1 1 d . . . H1S H 0.5965 0.6836 -0.0917 0.048 Uiso 1 1 calc R . . Cl1 Cl 0.54435(10) 0.87318(11) -0.06685(13) 0.0567(3) Uani 1 1 d . . . Cl2 Cl 0.43018(9) 0.66406(13) -0.12549(12) 0.0570(4) Uani 1 1 d . . . Cl3 Cl 0.55782(11) 0.68048(16) 0.10096(14) 0.0700(4) Uani 1 1 d . . . 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 0.0251(2) 0.0169(2) 0.0271(2) 0.00128(16) 0.00468(17) 0.00189(16) N1 0.0260(16) 0.0205(15) 0.0262(15) 0.0003(12) -0.0017(13) -0.0018(12) N2 0.0256(15) 0.0217(15) 0.0276(16) -0.0001(13) 0.0021(13) 0.0013(12) O1 0.0317(14) 0.0274(14) 0.0411(16) 0.0135(12) 0.0165(12) 0.0084(11) O2 0.0351(16) 0.0297(15) 0.0490(17) -0.0126(13) -0.0034(13) 0.0018(13) O3 0.0361(15) 0.0253(14) 0.0378(15) -0.0009(12) 0.0057(12) 0.0006(12) C1 0.0200(17) 0.0275(19) 0.0248(18) 0.0010(15) 0.0007(14) -0.0015(14) C2 0.0235(18) 0.0262(19) 0.0253(18) 0.0037(15) -0.0028(14) -0.0017(15) C3 0.031(2) 0.029(2) 0.0275(19) 0.0088(16) -0.0016(15) -0.0060(16) C4 0.030(2) 0.038(2) 0.0268(19) 0.0044(17) 0.0028(16) -0.0094(17) C5 0.0249(18) 0.035(2) 0.0263(19) -0.0083(16) 0.0055(15) -0.0046(16) C6 0.0263(18) 0.028(2) 0.0229(17) 0.0004(15) -0.0006(14) -0.0036(15) C7 0.044(2) 0.057(3) 0.034(2) 0.008(2) 0.0147(19) -0.008(2) C8 0.0266(18) 0.0198(18) 0.0297(19) 0.0059(15) -0.0044(15) -0.0022(14) C9 0.035(2) 0.0182(18) 0.032(2) -0.0011(15) -0.0049(16) 0.0029(15) C10 0.035(2) 0.0208(18) 0.032(2) -0.0033(15) 0.0037(16) 0.0057(16) C11 0.0254(18) 0.0262(19) 0.0250(18) -0.0048(15) 0.0024(15) 0.0026(15) C12 0.033(2) 0.029(2) 0.0268(19) 0.0005(16) 0.0058(16) -0.0039(17) C13 0.041(2) 0.038(2) 0.057(3) -0.012(2) -0.009(2) -0.005(2) C1S 0.032(2) 0.042(2) 0.046(2) -0.009(2) 0.0030(19) 0.0078(19) Cl1 0.0537(7) 0.0410(7) 0.0726(9) -0.0015(6) -0.0030(6) 0.0064(5) Cl2 0.0421(6) 0.0655(8) 0.0637(8) -0.0235(7) 0.0080(6) -0.0082(6) Cl3 0.0616(8) 0.0852(11) 0.0607(8) 0.0206(8) -0.0024(7) 0.0087(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 2.058(3) . y Zn1 N2 2.046(3) . y Zn1 O2 1.953(3) . y Zn1 O1 2.010(3) . y Zn1 O1 2.035(3) 3_565 y N1 C8 1.278(5) . ? N1 C9 1.476(5) . ? N2 C11 1.285(5) . ? N2 C10 1.460(5) . ? O1 C1 1.306(4) . ? O1 Zn1 2.035(3) 3_565 ? O2 C12 1.278(5) . ? O3 C12 1.233(5) . ? C1 C2 1.427(5) . ? C1 C6 1.427(5) . ? C2 C3 1.391(5) . ? C2 C8 1.465(5) . ? C3 C4 1.379(6) . ? C4 C5 1.395(6) . ? C4 C7 1.516(5) . ? C5 C6 1.395(5) . ? C6 C11 1.472(5) 3_565 ? C9 C10 1.538(6) . ? C12 C13 1.513(6) . ? C1S Cl1 1.770(5) . ? C1S Cl2 1.754(4) . ? C1S Cl3 1.760(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 O1 100.41(12) . .. Yes O2 Zn1 O1 104.71(13) . 3_565. Yes O1 Zn1 O1 76.22(11) . 3_565. Yes O2 Zn1 N2 117.70(12) . .. Yes O1 Zn1 N2 140.43(12) . .. Yes O1 Zn1 N2 83.79(11) 3_565 .. Yes O2 Zn1 N1 123.98(12) . .. Yes O1 Zn1 N1 84.91(12) . .. Yes O1 Zn1 N1 130.23(12) 3_565 .. Yes N2 Zn1 N1 82.49(12) . . ? C8 N1 C9 121.5(3) . . ? C8 N1 Zn1 126.0(3) . . ? C9 N1 Zn1 112.2(2) . . ? C11 N2 C10 122.8(3) . . ? C11 N2 Zn1 127.2(3) . . ? C10 N2 Zn1 109.6(2) . . ? C1 O1 Zn1 129.0(2) . . ? C1 O1 Zn1 126.5(2) . 3_565 ? Zn1 O1 Zn1 103.78(11) . 3_565 ? C12 O2 Zn1 113.2(2) . . ? O1 C1 C2 121.0(3) . . ? O1 C1 C6 120.1(3) . . ? C2 C1 C6 118.8(3) . . ? C3 C2 C1 118.9(3) . . ? C3 C2 C8 119.2(3) . . ? C1 C2 C8 121.5(3) . . ? C4 C3 C2 123.1(4) . . ? C3 C4 C5 117.7(3) . . ? C3 C4 C7 121.9(4) . . ? C5 C4 C7 120.4(4) . . ? C4 C5 C6 122.6(4) . . ? C5 C6 C1 118.8(3) . . ? C5 C6 C11 118.6(3) . 3_565 ? C1 C6 C11 122.5(3) . 3_565 ? N1 C8 C2 125.8(3) . . ? N1 C9 C10 111.2(3) . . ? N2 C10 C9 109.4(3) . . ? N2 C11 C6 124.0(3) . 3_565 ? O3 C12 O2 123.3(4) . . ? O3 C12 C13 119.9(4) . . ? O2 C12 C13 116.7(4) . . ? Cl2 C1S Cl3 111.5(3) . . ? Cl2 C1S Cl1 109.5(2) . . ? Cl3 C1S Cl1 109.2(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.71 _refine_diff_density_min -0.59 _refine_diff_density_rms 0.09 #===END data_2 _database_code_CSD 197069 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C28 H30 N4 O6 Zn2, 2(C H Cl3)' _chemical_formula_sum 'C30 H32 Cl6 N4 O6 Zn2' _chemical_formula_weight 888.04 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.416(2) _cell_length_b 9.184(2) _cell_length_c 14.217(3) _cell_angle_alpha 78.22(3) _cell_angle_beta 85.11(4) _cell_angle_gamma 82.28(3) _cell_volume 937.6(4) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 37 _cell_measurement_theta_min 14 _cell_measurement_theta_max 17 _exptl_crystal_description column _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method ? _exptl_crystal_F_000 450 _exptl_absorpt_coefficient_mu 1.752 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.762 _exptl_absorpt_correction_T_max 0.832 _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 'Stoe Stadi-4 four-circle' _diffrn_measurement_method omega-theta _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 'variations +-5.3' _diffrn_reflns_number 4857 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_av_sigmaI/netI 0.027 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3296 _reflns_number_observed 2961 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Stadi-4 (Stoe & Cie, 1995a)' _computing_cell_refinement 'Stadi-4 (Stoe & Cie, 1995a)' _computing_data_reduction 'X-Red (Stoe & Cie, 1995b)' _computing_structure_solution 'SHELXS-96 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2002)' _refine_special_details ; Refinement of F^2^ against ALL reflections. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.047P)^2^+1.700P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'methyl H atoms from difference Fourier; other placed geometrically' _refine_ls_hydrogen_treatment 'rigid rotating group; riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3296 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_obs 0.0398 _refine_ls_wR_factor_all 0.104 _refine_ls_wR_factor_obs 0.0974 _refine_ls_goodness_of_fit_all 1.061 _refine_ls_goodness_of_fit_obs 1.055 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.06563(5) 0.00843(4) 0.88490(2) 0.02325(13) Uani 1 1 d . . . O1 O 0.1376(3) -0.0937(3) 1.02387(15) 0.0260(5) Uani 1 1 d . . . O2 O -0.0713(3) -0.1429(3) 0.85075(16) 0.0277(5) Uani 1 1 d . . . O3 O 0.0917(4) -0.1276(3) 0.71193(18) 0.0420(6) Uani 1 1 d . . . N1 N 0.3419(4) -0.0056(3) 0.8439(2) 0.0292(6) Uani 1 1 d . . . N2 N -0.0015(4) 0.2031(3) 0.78226(19) 0.0278(6) Uani 1 1 d . . . C1 C 0.2824(4) -0.1896(4) 1.0475(2) 0.0253(7) Uani 1 1 d . . . C2 C 0.4427(4) -0.1922(4) 0.9853(2) 0.0294(7) Uani 1 1 d . . . C3 C 0.5944(5) -0.2983(4) 1.0102(3) 0.0374(9) Uani 1 1 d . . . H3 H 0.7016 -0.2949 0.9685 0.045 Uiso 1 1 calc R . . C4 C 0.5936(5) -0.4070(4) 1.0926(3) 0.0398(9) Uani 1 1 d . . . C5 C 0.4400(5) -0.4028(4) 1.1548(3) 0.0346(8) Uani 1 1 d . . . H5 H 0.4377 -0.4759 1.2127 0.042 Uiso 1 1 calc R . . C6 C 0.2865(5) -0.2947(4) 1.1361(2) 0.0285(7) Uani 1 1 d . . . C7 C 0.7583(6) -0.5239(5) 1.1155(4) 0.0534(11) Uani 1 1 d . . . H7A H 0.8626 -0.4741 1.1247 0.080 Uiso 1 1 calc R . . H7B H 0.7883 -0.5772 1.0620 0.080 Uiso 1 1 calc R . . H7C H 0.7301 -0.5954 1.1744 0.080 Uiso 1 1 calc R . . C8 C 0.4655(4) -0.0905(4) 0.8935(2) 0.0309(8) Uani 1 1 d . . . H8 H 0.5871 -0.0865 0.8670 0.037 Uiso 1 1 calc R . . C9 C 0.4084(5) 0.0704(5) 0.7476(3) 0.0378(9) Uani 1 1 d . . . H9A H 0.3931 0.0083 0.7002 0.045 Uiso 1 1 calc R . . H9B H 0.5404 0.0765 0.7488 0.045 Uiso 1 1 calc R . . C10 C 0.3132(5) 0.2259(4) 0.7141(3) 0.0368(8) Uani 1 1 d . . . H10A H 0.3799 0.2743 0.6552 0.044 Uiso 1 1 calc R . . H10B H 0.3185 0.2855 0.7643 0.044 Uiso 1 1 calc R . . C11 C 0.1149(5) 0.2296(4) 0.6927(2) 0.0332(8) Uani 1 1 d . . . H11A H 0.0724 0.3283 0.6534 0.040 Uiso 1 1 calc R . . H11B H 0.1046 0.1518 0.6550 0.040 Uiso 1 1 calc R . . C12 C -0.1450(5) 0.2973(4) 0.7868(2) 0.0302(7) Uani 1 1 d . . . C13 C -0.0308(4) -0.1772(4) 0.7688(2) 0.0273(7) Uani 1 1 d . . . C14 C -0.1459(5) -0.2843(5) 0.7411(3) 0.0414(9) Uani 1 1 d . . . H14A H -0.1684 -0.3634 0.7970 0.062 Uiso 1 1 calc R . . H14B H -0.0814 -0.3293 0.6890 0.062 Uiso 1 1 calc R . . H14C H -0.2625 -0.2296 0.7194 0.062 Uiso 1 1 calc R . . H1S H 0.214(6) -0.208(5) 0.588(3) 0.047(12) Uiso 1 1 d . . . C1S C 0.2786(6) -0.2309(5) 0.5384(3) 0.0447(10) Uani 1 1 d . . . Cl1 Cl 0.5102(2) -0.2357(2) 0.55585(12) 0.0960(6) Uani 1 1 d . . . Cl2 Cl 0.2267(3) -0.40382(15) 0.52011(12) 0.0917(5) Uani 1 1 d . . . Cl3 Cl 0.21463(18) -0.09286(14) 0.43855(8) 0.0595(3) Uani 1 1 d . . . 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 0.0187(2) 0.0309(2) 0.0210(2) -0.00664(15) 0.00174(14) -0.00529(15) O1 0.0198(11) 0.0343(13) 0.0235(11) -0.0082(9) -0.0015(9) 0.0024(9) O2 0.0239(11) 0.0333(13) 0.0285(12) -0.0111(10) 0.0016(9) -0.0074(10) O3 0.0535(17) 0.0448(15) 0.0328(14) -0.0153(12) 0.0109(12) -0.0209(13) N1 0.0227(14) 0.0422(17) 0.0255(14) -0.0113(12) 0.0042(11) -0.0097(12) N2 0.0282(15) 0.0321(15) 0.0246(14) -0.0048(11) 0.0007(11) -0.0115(12) C1 0.0217(16) 0.0297(17) 0.0284(17) -0.0137(13) -0.0055(13) -0.0023(13) C2 0.0195(16) 0.0394(19) 0.0334(18) -0.0166(15) -0.0042(13) -0.0018(14) C3 0.0244(18) 0.050(2) 0.042(2) -0.0216(18) -0.0057(15) 0.0011(16) C4 0.0299(19) 0.041(2) 0.053(2) -0.0221(18) -0.0126(17) 0.0076(16) C5 0.036(2) 0.0292(18) 0.041(2) -0.0086(15) -0.0159(16) -0.0020(15) C6 0.0279(17) 0.0269(17) 0.0339(18) -0.0096(14) -0.0092(14) -0.0046(14) C7 0.044(2) 0.045(2) 0.073(3) -0.023(2) -0.018(2) 0.0136(19) C8 0.0185(16) 0.048(2) 0.0300(18) -0.0175(16) 0.0044(13) -0.0059(15) C9 0.0252(18) 0.060(2) 0.0299(19) -0.0108(17) 0.0086(14) -0.0138(17) C10 0.038(2) 0.046(2) 0.0281(18) -0.0055(16) 0.0083(15) -0.0220(17) C11 0.041(2) 0.0358(19) 0.0234(17) -0.0018(14) 0.0009(14) -0.0134(16) C12 0.0347(19) 0.0272(17) 0.0320(18) -0.0074(14) -0.0073(14) -0.0104(15) C13 0.0272(17) 0.0255(16) 0.0284(17) -0.0046(13) -0.0044(14) 0.0003(13) C14 0.040(2) 0.044(2) 0.046(2) -0.0189(18) -0.0032(17) -0.0106(17) C1S 0.050(2) 0.052(2) 0.032(2) -0.0139(18) 0.0029(18) 0.0016(19) Cl1 0.0565(8) 0.1579(17) 0.0873(11) -0.0675(11) -0.0267(7) 0.0193(9) Cl2 0.1494(16) 0.0466(7) 0.0840(10) -0.0165(7) -0.0203(10) -0.0150(8) Cl3 0.0682(7) 0.0614(7) 0.0453(6) 0.0026(5) -0.0005(5) -0.0164(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 2.076(3) . ? Zn1 N2 2.096(3) . ? Zn1 O1 2.081(2) 2_557 ? Zn1 O1 2.087(2) . ? Zn1 O2 1.984(2) . ? O1 C1 1.315(4) . ? O1 Zn1 2.081(2) 2_557 ? O2 C13 1.269(4) . ? O3 C13 1.234(4) . ? N1 C8 1.280(5) . ? N1 C9 1.480(4) . ? N2 C12 1.284(5) . ? N2 C11 1.473(4) . ? C1 C2 1.421(5) . ? C1 C6 1.422(5) . ? C2 C3 1.405(5) . ? C2 C8 1.453(5) . ? C3 C4 1.376(6) . ? C4 C5 1.383(6) . ? C4 C7 1.524(5) . ? C5 C6 1.412(5) . ? C6 C12 1.450(5) 2_557 ? C9 C10 1.508(6) . ? C10 C11 1.522(5) . ? C12 C6 1.450(5) 2_557 ? C13 C14 1.515(5) . ? C1S Cl1 1.749(5) . ? C1S Cl2 1.758(5) . ? C1S Cl3 1.751(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 N1 116.53(10) . . ? O2 Zn1 O1 97.07(9) . 2_557 ? N1 Zn1 O1 144.76(10) . 2_557 ? O2 Zn1 O1 101.57(10) . . ? N1 Zn1 O1 87.70(11) . . ? O1 Zn1 O1 74.74(10) 2_557 . ? O2 Zn1 N2 104.44(10) . . ? N1 Zn1 N2 94.02(12) . . ? O1 Zn1 N2 87.16(10) 2_557 . ? O1 Zn1 N2 149.88(10) . . ? C1 O1 Zn1 128.0(2) . 2_557 ? C1 O1 Zn1 126.7(2) . . ? Zn1 O1 Zn1 105.26(10) 2_557 . ? C13 O2 Zn1 116.8(2) . . ? C8 N1 C9 114.4(3) . . ? C8 N1 Zn1 124.1(2) . . ? C9 N1 Zn1 121.2(2) . . ? C12 N2 C11 115.9(3) . . ? C12 N2 Zn1 125.6(2) . . ? C11 N2 Zn1 118.3(2) . . ? O1 C1 C2 121.1(3) . . ? O1 C1 C6 121.9(3) . . ? C2 C1 C6 117.0(3) . . ? C3 C2 C1 120.5(3) . . ? C3 C2 C8 114.8(3) . . ? C1 C2 C8 124.7(3) . . ? C4 C3 C2 122.5(4) . . ? C3 C4 C5 117.3(3) . . ? C3 C4 C7 121.0(4) . . ? C5 C4 C7 121.6(4) . . ? C4 C5 C6 122.8(4) . . ? C5 C6 C1 119.6(3) . . ? C5 C6 C12 115.6(3) . 2_557 ? C1 C6 C12 124.8(3) . 2_557 ? N1 C8 C2 128.0(3) . . ? N1 C9 C10 114.5(3) . . ? C9 C10 C11 114.0(3) . . ? N2 C11 C10 111.0(3) . . ? N2 C12 C6 127.6(3) . 2_557 ? O3 C13 O2 124.4(3) . . ? O3 C13 C14 119.6(3) . . ? O2 C13 C14 116.0(3) . . ? Cl1 C1S Cl3 110.4(3) . . ? Cl1 C1S Cl2 111.8(3) . . ? Cl3 C1S Cl2 108.5(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.73 _refine_diff_density_min -0.61 _refine_diff_density_rms 0.08 #===END data_4 _database_code_CSD 197070 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H35 N5 O2 Zn 2+, 2(P F6 -)' _chemical_formula_sum 'C28 H35 F12 N5 O2 P2 Zn' _chemical_formula_weight 828.92 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' F F 0.0171 0.0103 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.34(2) _cell_length_b 19.998(7) _cell_length_c 21.537(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6607(10) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 44 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 17.0 _exptl_crystal_description 'irregular block' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.667 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3376 _exptl_absorpt_coefficient_mu 0.945 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.455 _exptl_absorpt_correction_T_max 0.546 _exptl_absorpt_process_details 'X-RED (Stoe, 1995)' _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 9.0 _diffrn_reflns_number 6612 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_av_sigmaI/netI 0.035 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5804 _reflns_number_gt 4633 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI4 (Stoe, 1995)' _computing_cell_refinement STADI4 _computing_data_reduction 'X-RED (Stoe, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2002)' _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^)+(0.049P)^2^+39.50P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'difference map or placed geometrically' _refine_ls_hydrogen_treatment 'methyl H atoms in rigid group, N-H with distance restraint; others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5799 _refine_ls_number_parameters 474 _refine_ls_number_restraints 110 _refine_ls_R_factor_all 0.0938 _refine_ls_R_factor_gt 0.0709 _refine_ls_wR_factor_ref 0.177 _refine_ls_wR_factor_gt 0.155 _refine_ls_goodness_of_fit_ref 1.160 _refine_ls_restrained_S_all 1.170 _refine_ls_shift/su_max 0.005 _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 0.86546(4) 0.09848(3) 0.52210(3) 0.0187(2) Uani 0.899(2) 1 d P A 1 Zn2 Zn 0.8366(4) 0.1141(3) 0.4203(3) 0.026(2) Uani 0.101(2) 1 d P A 2 O1 O 0.9087(3) 0.17338(17) 0.47085(17) 0.0255(8) Uani 1 1 d . . . O2 O 0.8943(3) 0.04089(17) 0.45088(17) 0.0249(8) Uani 1 1 d . . . N1S N 0.7335(3) 0.1102(2) 0.5180(2) 0.0360(12) Uani 1 1 d . . . C1S C 0.6605(4) 0.1149(3) 0.5229(3) 0.0358(15) Uani 1 1 d . A . C2S C 0.5683(4) 0.1191(3) 0.5305(4) 0.0444(17) Uani 1 1 d . . . H2S1 H 0.5495 0.0870 0.5622 0.067 Uiso 1 1 calc R A . H2S2 H 0.5397 0.1086 0.4910 0.067 Uiso 1 1 calc R . . H2S3 H 0.5524 0.1644 0.5435 0.067 Uiso 1 1 calc R . . N1 N 0.9044(3) 0.1526(2) 0.5977(2) 0.0248(10) Uani 1 1 d . . . N2 N 0.8834(3) 0.0172(2) 0.5779(2) 0.0245(10) Uani 1 1 d . . . N3 N 0.8467(3) 0.0559(2) 0.3392(2) 0.0269(11) Uani 1 1 d D . . H3N H 0.860(4) 0.065(3) 0.3751(11) 0.032 Uiso 1 1 d D . . N4 N 0.8814(4) 0.1998(2) 0.3588(2) 0.0304(11) Uani 1 1 d D . . H4N H 0.886(4) 0.175(3) 0.3892(18) 0.036 Uiso 1 1 d D . . C1 C 0.8947(3) 0.2368(2) 0.4849(2) 0.0208(11) Uani 1 1 d . A . C2 C 0.8976(3) 0.2596(3) 0.5474(2) 0.0229(11) Uani 1 1 d . . . C3 C 0.8788(3) 0.3272(3) 0.5586(3) 0.0267(12) Uani 1 1 d . A . H3B H 0.8796 0.3426 0.6004 0.032 Uiso 1 1 calc R . . C4 C 0.8591(3) 0.3726(3) 0.5122(3) 0.0264(12) Uani 1 1 d . . . C5 C 0.8611(3) 0.3502(3) 0.4518(3) 0.0269(12) Uani 1 1 d . A . H5A H 0.8499 0.3811 0.4193 0.032 Uiso 1 1 calc R . . C6 C 0.8788(3) 0.2837(3) 0.4364(2) 0.0210(11) Uani 1 1 d . . . C7 C 0.8405(4) 0.4451(3) 0.5274(3) 0.0404(16) Uani 1 1 d . A . H7A H 0.7907 0.4478 0.5558 0.061 Uiso 1 1 calc R . . H7B H 0.8268 0.4694 0.4890 0.061 Uiso 1 1 calc R . . H7C H 0.8918 0.4652 0.5470 0.061 Uiso 1 1 calc R . . C8 C 0.9183(4) 0.2163(3) 0.6003(2) 0.0255(12) Uani 1 1 d . A . C9 C 0.9544(5) 0.2476(3) 0.6578(3) 0.0424(16) Uani 1 1 d . . . H9A H 0.9808 0.2908 0.6474 0.064 Uiso 1 1 calc R A . H9B H 0.9987 0.2182 0.6759 0.064 Uiso 1 1 calc R . . H9C H 0.9073 0.2544 0.6880 0.064 Uiso 1 1 calc R . . C10 C 0.9220(4) 0.1084(3) 0.6504(2) 0.0277(12) Uani 1 1 d . A . H10A H 0.9022 0.1300 0.6893 0.033 Uiso 1 1 calc R . . H10B H 0.9856 0.1004 0.6538 0.033 Uiso 1 1 calc R . . C11 C 0.8750(4) 0.0421(3) 0.6420(2) 0.0306(13) Uani 1 1 d . A . H11A H 0.8996 0.0088 0.6711 0.037 Uiso 1 1 calc R . . H11B H 0.8125 0.0479 0.6522 0.037 Uiso 1 1 calc R . . C12 C 0.8970(3) -0.0444(3) 0.5642(3) 0.0247(12) Uani 1 1 d . A . C13 C 0.9165(5) -0.0958(3) 0.6132(3) 0.0396(15) Uani 1 1 d . . . H13A H 0.9428 -0.0739 0.6493 0.059 Uiso 1 1 calc R A . H13B H 0.9570 -0.1291 0.5964 0.059 Uiso 1 1 calc R . . H13C H 0.8622 -0.1180 0.6257 0.059 Uiso 1 1 calc R . . C14 C 0.8880(3) -0.0676(3) 0.4984(3) 0.0219(11) Uani 1 1 d . . . C15 C 0.8779(3) -0.1364(3) 0.4887(3) 0.0255(12) Uani 1 1 d . A . H15A H 0.8838 -0.1655 0.5233 0.031 Uiso 1 1 calc R . . C16 C 0.8596(4) -0.1640(3) 0.4310(3) 0.0268(12) Uani 1 1 d . . . C17 C 0.8496(3) -0.1212(3) 0.3811(3) 0.0263(12) Uani 1 1 d . A . H17A H 0.8359 -0.1395 0.3416 0.032 Uiso 1 1 calc R . . C18 C 0.8589(3) -0.0513(3) 0.3869(2) 0.0219(11) Uani 1 1 d . . . C19 C 0.8801(3) -0.0238(2) 0.4463(2) 0.0204(11) Uani 1 1 d . A . C20 C 0.8483(4) -0.2388(3) 0.4245(3) 0.0362(15) Uani 1 1 d . A . H20A H 0.9027 -0.2613 0.4361 0.054 Uiso 1 1 calc R . . H20B H 0.8339 -0.2496 0.3813 0.054 Uiso 1 1 calc R . . H20C H 0.8011 -0.2539 0.4517 0.054 Uiso 1 1 calc R . . C21 C 0.8416(3) -0.0089(3) 0.3330(2) 0.0220(11) Uani 1 1 d . A . C22 C 0.8164(5) -0.0382(3) 0.2716(3) 0.0381(15) Uani 1 1 d . . . H22A H 0.8118 -0.0024 0.2407 0.057 Uiso 1 1 calc R A . H22B H 0.7601 -0.0609 0.2755 0.057 Uiso 1 1 calc R . . H22C H 0.8608 -0.0704 0.2584 0.057 Uiso 1 1 calc R . . C23 C 0.8219(4) 0.1072(3) 0.2942(3) 0.0301(13) Uani 1 1 d . A . H23A H 0.7612 0.1215 0.3024 0.036 Uiso 1 1 calc R . . H23B H 0.8241 0.0880 0.2519 0.036 Uiso 1 1 calc R . . C24 C 0.8817(4) 0.1680(3) 0.2973(2) 0.0336(14) Uani 1 1 d . A . H24A H 0.9419 0.1540 0.2870 0.040 Uiso 1 1 calc R . . H24B H 0.8629 0.2010 0.2658 0.040 Uiso 1 1 calc R . . C25 C 0.8786(4) 0.2628(3) 0.3711(3) 0.0269(12) Uani 1 1 d . A . C26 C 0.8788(5) 0.3128(3) 0.3197(3) 0.0395(15) Uani 1 1 d . . . H26A H 0.8844 0.3579 0.3371 0.059 Uiso 1 1 calc R A . H26B H 0.8241 0.3095 0.2964 0.059 Uiso 1 1 calc R . . H26C H 0.9279 0.3039 0.2918 0.059 Uiso 1 1 calc R . . P1 P 0.66205(11) 0.23007(8) 0.68835(8) 0.0382(4) Uani 1 1 d DU . . F1 F 0.7252(3) 0.2926(2) 0.6871(3) 0.0787(15) Uani 1 1 d DU . . F2 F 0.6518(6) 0.2385(3) 0.6168(2) 0.124(3) Uani 1 1 d DU . . F3 F 0.7430(4) 0.1824(3) 0.6814(3) 0.0932(19) Uani 1 1 d DU . . F4 F 0.5846(3) 0.2799(3) 0.6995(3) 0.096(2) Uani 1 1 d DU . . F5 F 0.6755(5) 0.2239(3) 0.7606(2) 0.112(2) Uani 1 1 d DU . . F6 F 0.6008(4) 0.1687(3) 0.6917(5) 0.157(4) Uani 1 1 d DU . . P2 P 0.55640(14) 0.03437(9) 0.33156(8) 0.0450(5) Uani 1 1 d U . . F21 F 0.6459(4) 0.0000(3) 0.3496(4) 0.123(2) Uani 1 1 d DU . . F22 F 0.5834(5) 0.0980(3) 0.3696(3) 0.134(3) Uani 1 1 d DU . . F23 F 0.5191(5) 0.0035(5) 0.3903(4) 0.164(4) Uani 1 1 d DU . . F24 F 0.6043(5) 0.0656(4) 0.2745(3) 0.142(3) Uani 1 1 d DU . . F25 F 0.5326(5) -0.0282(3) 0.2927(4) 0.150(3) Uani 1 1 d DU . . F26 F 0.4690(4) 0.0689(3) 0.3166(4) 0.138(3) Uani 1 1 d DU . . 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 0.0223(4) 0.0178(3) 0.0160(3) 0.0019(3) 0.0004(3) 0.0019(3) Zn2 0.033(4) 0.025(4) 0.020(3) 0.005(3) 0.005(3) -0.011(3) O1 0.037(2) 0.0161(18) 0.0236(19) -0.0015(15) 0.0047(17) -0.0009(16) O2 0.033(2) 0.0183(18) 0.0234(19) -0.0014(15) 0.0001(16) -0.0036(16) N1S 0.033(3) 0.030(3) 0.045(3) 0.003(2) -0.003(2) 0.002(2) C1S 0.026(3) 0.024(3) 0.058(4) 0.002(3) -0.003(3) 0.002(2) C2S 0.026(3) 0.044(4) 0.064(5) 0.004(3) 0.002(3) -0.002(3) N1 0.030(2) 0.026(2) 0.019(2) 0.0015(19) 0.0030(19) 0.003(2) N2 0.031(3) 0.022(2) 0.020(2) 0.0014(19) 0.0007(19) 0.001(2) N3 0.040(3) 0.023(2) 0.018(2) 0.001(2) -0.002(2) -0.002(2) N4 0.047(3) 0.025(3) 0.019(2) 0.003(2) -0.003(2) 0.003(2) C1 0.017(2) 0.019(3) 0.027(3) -0.003(2) 0.003(2) -0.001(2) C2 0.022(3) 0.021(3) 0.025(3) -0.002(2) 0.004(2) -0.006(2) C3 0.021(3) 0.028(3) 0.031(3) -0.009(2) 0.002(2) -0.003(2) C4 0.019(3) 0.020(3) 0.040(3) -0.005(2) -0.001(2) 0.001(2) C5 0.021(3) 0.023(3) 0.037(3) 0.002(2) -0.005(2) 0.001(2) C6 0.015(2) 0.024(3) 0.024(3) 0.001(2) 0.001(2) -0.002(2) C7 0.035(3) 0.025(3) 0.061(4) -0.016(3) -0.011(3) 0.007(3) C8 0.026(3) 0.031(3) 0.019(3) -0.003(2) 0.009(2) 0.001(2) C9 0.059(4) 0.041(4) 0.027(3) -0.005(3) -0.002(3) -0.009(3) C10 0.035(3) 0.032(3) 0.016(3) 0.000(2) 0.002(2) 0.004(3) C11 0.045(4) 0.030(3) 0.017(3) 0.002(2) 0.005(3) 0.004(3) C12 0.020(3) 0.026(3) 0.028(3) 0.009(2) 0.005(2) 0.001(2) C13 0.058(4) 0.029(3) 0.032(3) 0.010(3) 0.001(3) 0.014(3) C14 0.018(3) 0.019(3) 0.028(3) 0.002(2) 0.003(2) 0.000(2) C15 0.023(3) 0.023(3) 0.031(3) 0.005(2) 0.002(2) 0.000(2) C16 0.022(3) 0.018(3) 0.040(3) 0.003(2) 0.002(2) -0.002(2) C17 0.022(3) 0.022(3) 0.035(3) -0.006(2) 0.000(2) 0.000(2) C18 0.018(3) 0.019(2) 0.029(3) 0.002(2) 0.005(2) 0.002(2) C19 0.016(3) 0.018(3) 0.027(3) 0.003(2) 0.003(2) 0.003(2) C20 0.032(3) 0.025(3) 0.052(4) 0.002(3) -0.006(3) 0.002(3) C21 0.020(3) 0.022(3) 0.024(3) -0.004(2) 0.002(2) -0.002(2) C22 0.058(4) 0.029(3) 0.027(3) -0.004(3) 0.000(3) -0.005(3) C23 0.044(4) 0.024(3) 0.022(3) 0.003(2) -0.005(3) 0.001(3) C24 0.058(4) 0.025(3) 0.018(3) 0.006(2) 0.004(3) 0.000(3) C25 0.024(3) 0.029(3) 0.028(3) 0.007(2) -0.001(2) 0.000(2) C26 0.058(4) 0.031(3) 0.029(3) 0.006(3) 0.001(3) -0.005(3) P1 0.0334(9) 0.0371(9) 0.0443(10) 0.0168(8) 0.0007(7) 0.0070(7) F1 0.066(3) 0.065(3) 0.105(4) 0.021(3) -0.014(3) -0.017(3) F2 0.247(9) 0.068(3) 0.057(3) 0.000(3) -0.061(4) 0.011(4) F3 0.091(4) 0.087(4) 0.102(4) 0.024(3) 0.035(3) 0.052(3) F4 0.067(3) 0.074(3) 0.147(5) 0.062(4) 0.044(3) 0.037(3) F5 0.169(6) 0.118(5) 0.049(3) 0.038(3) 0.022(3) 0.065(4) F6 0.086(4) 0.070(4) 0.315(11) 0.100(5) -0.072(6) -0.033(3) P2 0.0614(12) 0.0334(9) 0.0402(10) 0.0074(8) 0.0104(9) 0.0095(8) F21 0.063(4) 0.120(5) 0.185(7) 0.016(5) 0.020(4) 0.031(4) F22 0.198(8) 0.087(4) 0.116(5) -0.046(4) -0.044(5) 0.019(5) F23 0.140(6) 0.192(7) 0.159(6) 0.117(6) 0.095(6) 0.049(6) F24 0.206(8) 0.150(6) 0.071(4) 0.025(4) 0.036(5) -0.051(6) F25 0.158(7) 0.080(4) 0.212(8) -0.063(5) -0.024(6) -0.013(4) F26 0.119(5) 0.098(5) 0.199(8) -0.001(5) -0.074(5) 0.049(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 2.045(5) . ? Zn1 N2 2.040(4) . ? Zn1 N1S 2.040(6) . ? Zn1 O1 1.976(4) . ? Zn1 O2 1.969(4) . ? Zn2 N3 2.106(8) . ? Zn2 N4 2.272(7) . ? Zn2 O1 1.953(7) . ? Zn2 O2 1.833(7) . ? O1 C1 1.322(6) . ? O2 C19 1.315(6) . ? N1S C1S 1.128(8) . ? C1S C2S 1.426(9) . ? N1 C8 1.291(7) . ? N1 C10 1.465(7) . ? N2 C12 1.283(7) . ? N2 C11 1.475(7) . ? N3 C21 1.306(7) . ? N3 C23 1.460(7) . ? N4 C25 1.290(7) . ? N4 C24 1.470(7) . ? C1 C2 1.421(7) . ? C1 C6 1.424(7) . ? C2 C3 1.403(7) . ? C2 C8 1.468(8) . ? C3 C4 1.384(8) . ? C4 C5 1.377(8) . ? C4 C7 1.514(7) . ? C5 C6 1.398(7) . ? C6 C25 1.468(8) . ? C8 C9 1.495(8) . ? C10 C11 1.520(8) . ? C12 C14 1.496(8) . ? C12 C13 1.504(7) . ? C14 C15 1.400(7) . ? C14 C19 1.429(7) . ? C15 C16 1.388(8) . ? C16 C17 1.383(8) . ? C16 C20 1.512(7) . ? C17 C18 1.410(7) . ? C18 C19 1.430(7) . ? C18 C21 1.462(7) . ? C21 C22 1.497(8) . ? C23 C24 1.524(8) . ? C25 C26 1.491(8) . ? P1 F1 1.582(5) . ? P1 F2 1.557(5) . ? P1 F3 1.572(5) . ? P1 F4 1.568(5) . ? P1 F5 1.575(5) . ? P1 F6 1.547(5) . ? P2 F21 1.584(6) . ? P2 F22 1.569(6) . ? P2 F23 1.520(6) . ? P2 F24 1.563(6) . ? P2 F25 1.549(6) . ? P2 F26 1.543(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 O1 86.13(15) . . ? O2 Zn1 N2 87.84(17) . . ? O1 Zn1 N2 152.63(18) . . ? O2 Zn1 N1S 104.88(19) . . ? O1 Zn1 N1S 102.82(19) . . ? N2 Zn1 N1S 104.53(19) . . ? O2 Zn1 N1 149.86(18) . . ? O1 Zn1 N1 86.86(17) . . ? N2 Zn1 N1 85.07(18) . . ? N1S Zn1 N1 105.3(2) . . ? O2 Zn2 O1 90.6(3) . . ? O2 Zn2 N3 79.7(3) . . ? O1 Zn2 N3 139.1(4) . . ? O2 Zn2 N4 131.7(4) . . ? O1 Zn2 N4 72.3(3) . . ? N3 Zn2 N4 84.8(3) . . ? C1 O1 Zn2 128.2(4) . . ? C1 O1 Zn1 123.0(3) . . ? Zn2 O1 Zn1 70.1(2) . . ? C19 O2 Zn2 132.7(4) . . ? C19 O2 Zn1 126.6(3) . . ? Zn2 O2 Zn1 72.8(2) . . ? C1S N1S Zn1 171.9(6) . . ? N1S C1S C2S 178.1(7) . . ? C8 N1 C10 122.0(5) . . ? C8 N1 Zn1 127.2(4) . . ? C10 N1 Zn1 110.6(3) . . ? C12 N2 C11 123.7(5) . . ? C12 N2 Zn1 130.6(4) . . ? C11 N2 Zn1 105.7(3) . . ? C21 N3 C23 127.9(5) . . ? C21 N3 Zn2 129.0(4) . . ? C23 N3 Zn2 98.3(4) . . ? C25 N4 C24 127.4(5) . . ? C25 N4 Zn2 127.5(4) . . ? C24 N4 Zn2 101.6(4) . . ? O1 C1 C2 121.3(5) . . ? O1 C1 C6 119.4(5) . . ? C2 C1 C6 119.3(4) . . ? C3 C2 C1 117.8(5) . . ? C3 C2 C8 118.6(5) . . ? C1 C2 C8 123.6(5) . . ? C4 C3 C2 123.5(5) . . ? C5 C4 C3 117.7(5) . . ? C5 C4 C7 121.3(5) . . ? C3 C4 C7 121.0(5) . . ? C4 C5 C6 122.5(5) . . ? C5 C6 C1 119.1(5) . . ? C5 C6 C25 119.8(5) . . ? C1 C6 C25 121.1(5) . . ? N1 C8 C2 120.8(5) . . ? N1 C8 C9 120.7(5) . . ? C2 C8 C9 118.5(5) . . ? N1 C10 C11 110.3(4) . . ? N2 C11 C10 111.4(4) . . ? N2 C12 C14 120.0(5) . . ? N2 C12 C13 121.8(5) . . ? C14 C12 C13 118.1(5) . . ? C15 C14 C19 118.4(5) . . ? C15 C14 C12 117.1(5) . . ? C19 C14 C12 124.2(5) . . ? C16 C15 C14 123.2(5) . . ? C17 C16 C15 118.1(5) . . ? C17 C16 C20 121.8(5) . . ? C15 C16 C20 120.1(5) . . ? C16 C17 C18 122.3(5) . . ? C17 C18 C19 118.9(5) . . ? C17 C18 C21 119.1(5) . . ? C19 C18 C21 121.9(4) . . ? O2 C19 C14 121.9(5) . . ? O2 C19 C18 118.9(5) . . ? C14 C19 C18 119.1(5) . . ? N3 C21 C18 119.0(5) . . ? N3 C21 C22 119.6(5) . . ? C18 C21 C22 121.5(5) . . ? N3 C23 C24 112.0(5) . . ? N4 C24 C23 112.5(5) . . ? N4 C25 C6 118.3(5) . . ? N4 C25 C26 120.2(5) . . ? C6 C25 C26 121.4(5) . . ? F6 P1 F2 94.1(5) . . ? F6 P1 F4 92.1(4) . . ? F2 P1 F4 90.4(4) . . ? F6 P1 F3 90.2(4) . . ? F2 P1 F3 93.0(4) . . ? F4 P1 F3 175.8(4) . . ? F6 P1 F5 88.3(5) . . ? F2 P1 F5 177.6(4) . . ? F4 P1 F5 89.8(3) . . ? F3 P1 F5 86.7(3) . . ? F6 P1 F1 178.2(4) . . ? F2 P1 F1 87.7(3) . . ? F4 P1 F1 88.0(3) . . ? F3 P1 F1 89.6(3) . . ? F5 P1 F1 89.9(4) . . ? F23 P2 F26 91.7(4) . . ? F23 P2 F25 91.8(5) . . ? F26 P2 F25 92.5(4) . . ? F23 P2 F24 174.0(5) . . ? F26 P2 F24 93.7(4) . . ? F25 P2 F24 90.5(4) . . ? F23 P2 F22 89.6(5) . . ? F26 P2 F22 88.6(4) . . ? F25 P2 F22 178.1(5) . . ? F24 P2 F22 87.9(4) . . ? F23 P2 F21 86.9(4) . . ? F26 P2 F21 177.8(4) . . ? F25 P2 F21 89.2(4) . . ? F24 P2 F21 87.6(4) . . ? F22 P2 F21 89.7(4) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.16 _refine_diff_density_min -0.54 _refine_diff_density_rms 0.10 #===END data_5 _database_code_CSD 197071 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C26 H29 N4 O4 P Zn2 +, P F6 -, C2 H3 N' _chemical_formula_sum 'C28 H32 F6 N5 O4 P Zn2' _chemical_formula_weight 778.30 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' F F 0.0171 0.0103 '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' Zn Zn 0.2839 1.4301 '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 15.736(4) _cell_length_b 12.177(5) _cell_length_c 16.237(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.85(2) _cell_angle_gamma 90.00 _cell_volume 3074.2(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 26 _cell_measurement_theta_min 12.65 _cell_measurement_theta_max 16.3 _exptl_crystal_description orange _exptl_crystal_colour 'thick plate' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 1.693 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.727 _exptl_absorpt_correction_T_max 0.958 _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 'Stoe Stadi-4' _diffrn_measurement_method Omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 'random variation +- 2.05' _diffrn_reflns_number 7222 _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_av_sigmaI/netI 0.034 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -2 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 25.0 _reflns_number_total 5411 _reflns_number_gt 4401 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI-4 (Stoe, 1995)' _computing_cell_refinement STADI-4 _computing_data_reduction 'X-RED (Stoe, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2002)' _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 w=1/[\s^2^(Fo^2^)+(0.018P)^2^+10.11P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'difference Fourier; geometrically placed' _refine_ls_hydrogen_treatment 'rigid rotating group; riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5411 _refine_ls_number_parameters 436 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.0659 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.101 _refine_ls_wR_factor_gt 0.0868 _refine_ls_goodness_of_fit_ref 1.171 _refine_ls_restrained_S_all 1.169 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.56625(3) 0.68490(4) 0.05293(3) 0.02127(13) Uani 1 d . . . Zn2 Zn 0.69044(3) 0.66511(4) -0.07219(3) 0.02217(13) Uani 1 d . . . O1 O 0.56370(17) 0.6284(2) -0.06790(17) 0.0225(6) Uani 1 d . . . O2 O 0.68824(18) 0.6293(2) 0.05263(17) 0.0233(7) Uani 1 d . . . N1 N 0.4394(2) 0.6466(3) 0.0410(2) 0.0252(8) Uani 1 d . . . N2 N 0.5897(2) 0.6892(3) 0.1810(2) 0.0253(8) Uani 1 d . . . N3 N 0.6658(2) 0.6412(3) -0.1979(2) 0.0254(8) Uani 1 d . . . N4 N 0.8147(2) 0.6082(3) -0.0564(2) 0.0245(8) Uani 1 d . . . C1 C 0.4979(3) 0.6227(3) -0.1280(3) 0.0233(9) Uani 1 d . . . C2 C 0.4122(3) 0.6185(3) -0.1106(3) 0.0220(9) Uani 1 d . . . C3 C 0.3428(3) 0.6079(3) -0.1764(3) 0.0248(10) Uani 1 d . . . H3 H 0.2861 0.6048 -0.1634 0.030 Uiso 1 calc R . . C4 C 0.3541(3) 0.6019(3) -0.2590(3) 0.0251(10) Uani 1 d . . . C5 C 0.4377(3) 0.6082(4) -0.2753(3) 0.0262(10) Uani 1 d . . . H5 H 0.4470 0.6051 -0.3317 0.031 Uiso 1 calc R . . C6 C 0.5095(3) 0.6189(3) -0.2128(3) 0.0226(9) Uani 1 d . . . C7 C 0.2796(3) 0.5905(4) -0.3294(3) 0.0307(11) Uani 1 d . . . H7A H 0.2253 0.5933 -0.3068 0.046 Uiso 1 calc R . . H7B H 0.2839 0.5202 -0.3578 0.046 Uiso 1 calc R . . H7C H 0.2812 0.6508 -0.3691 0.046 Uiso 1 calc R . . C8 C 0.3893(3) 0.6261(3) -0.0276(3) 0.0244(9) Uani 1 d . . . H8 H 0.3304 0.6145 -0.0234 0.029 Uiso 1 calc R . . C9 C 0.3993(3) 0.6529(4) 0.1172(3) 0.0336(11) Uani 1 d . . . H9A H 0.4088 0.5831 0.1484 0.040 Uiso 1 calc R . . H9B H 0.3365 0.6638 0.1017 0.040 Uiso 1 calc R . . C10 C 0.4372(3) 0.7473(4) 0.1721(3) 0.0320(11) Uani 1 d . . . H10A H 0.4474 0.8098 0.1358 0.038 Uiso 1 calc R . . H10B H 0.3943 0.7713 0.2070 0.038 Uiso 1 calc R . . C11 C 0.5199(3) 0.7212(4) 0.2281(3) 0.0354(12) Uani 1 d . . . H11A H 0.5384 0.7864 0.2628 0.043 Uiso 1 calc R . . H11B H 0.5097 0.6606 0.2660 0.043 Uiso 1 calc R . . C12 C 0.6626(3) 0.6706(4) 0.2256(3) 0.0248(9) Uani 1 d . . . H12 H 0.6645 0.6778 0.2841 0.030 Uiso 1 calc R . . C13 C 0.7428(3) 0.6399(3) 0.1982(3) 0.0236(9) Uani 1 d . . . C14 C 0.8137(3) 0.6283(4) 0.2610(3) 0.0285(10) Uani 1 d . . . H14 H 0.8058 0.6416 0.3170 0.034 Uiso 1 calc R . . C15 C 0.8946(3) 0.5984(4) 0.2462(3) 0.0317(11) Uani 1 d . . . C16 C 0.9046(3) 0.5844(4) 0.1638(3) 0.0316(11) Uani 1 d . . . H16 H 0.9597 0.5649 0.1516 0.038 Uiso 1 calc R . . C17 C 0.8367(3) 0.5976(4) 0.0971(3) 0.0244(9) Uani 1 d . . . C18 C 0.7534(3) 0.6230(3) 0.1138(3) 0.0220(9) Uani 1 d . . . C19 C 0.9680(3) 0.5816(5) 0.3165(3) 0.0450(14) Uani 1 d . . . H19A H 0.9634 0.6347 0.3610 0.067 Uiso 1 calc R . . H19B H 1.0227 0.5924 0.2958 0.067 Uiso 1 calc R . . H19C H 0.9656 0.5069 0.3385 0.067 Uiso 1 calc R . . C20 C 0.8595(3) 0.5846(4) 0.0147(3) 0.0270(10) Uani 1 d . . . H20 H 0.9149 0.5546 0.0127 0.032 Uiso 1 calc R . . C21 C 0.8616(3) 0.5918(4) -0.1284(3) 0.0328(11) Uani 1 d . . . H21A H 0.9069 0.5359 -0.1133 0.039 Uiso 1 calc R . . H21B H 0.8903 0.6615 -0.1394 0.039 Uiso 1 calc R . . C22 C 0.8050(3) 0.5561(4) -0.2072(3) 0.0342(11) Uani 1 d . . . H22A H 0.7740 0.4885 -0.1955 0.041 Uiso 1 calc R . . H22B H 0.8418 0.5377 -0.2495 0.041 Uiso 1 calc R . . C23 C 0.7396(3) 0.6423(4) -0.2433(3) 0.0341(11) Uani 1 d . . . H23A H 0.7668 0.7158 -0.2388 0.041 Uiso 1 calc R . . H23B H 0.7199 0.6267 -0.3030 0.041 Uiso 1 calc R . . C24 C 0.5916(3) 0.6269(4) -0.2413(3) 0.0244(10) Uani 1 d . . . H24 H 0.5904 0.6208 -0.2998 0.029 Uiso 1 calc R . . C25 C 0.6333(3) 0.8829(4) -0.0183(3) 0.0260(10) Uani 1 d . . . C26 C 0.6368(3) 1.0062(4) -0.0256(3) 0.0321(11) Uani 1 d . . . H26A H 0.5800 1.0371 -0.0219 0.048 Uiso 1 calc R . . H26B H 0.6536 1.0260 -0.0794 0.048 Uiso 1 calc R . . H26C H 0.6790 1.0356 0.0197 0.048 Uiso 1 calc R . . O3 O 0.58065(19) 0.8438(2) 0.02431(18) 0.0262(7) Uani 1 d . . . O4 O 0.68348(19) 0.8282(3) -0.05671(19) 0.0286(7) Uani 1 d . . . P P 0.87276(8) 0.25140(11) 0.01015(8) 0.0327(3) Uani 1 d D . . F1 F 0.8338(3) 0.3431(3) -0.0519(3) 0.0933(15) Uani 1 d D . . F2 F 0.7862(4) 0.1893(5) -0.0186(5) 0.128(3) Uani 0.849(8) d PD A 1 F3 F 0.9103(4) 0.1824(5) -0.0580(2) 0.091(2) Uani 0.849(8) d PD A 1 F4 F 0.9575(3) 0.3147(5) 0.0345(4) 0.109(2) Uani 0.849(8) d PD A 1 F5 F 0.8337(4) 0.3159(5) 0.0787(3) 0.092(2) Uani 0.849(8) d PD A 1 F2' F 0.8342(15) 0.1595(14) -0.0508(11) 0.039(6) Uiso 0.151(8) d PD A 2 F3' F 0.9495(12) 0.264(2) -0.0384(14) 0.054(7) Uiso 0.151(8) d PD A 2 F4' F 0.9102(18) 0.3346(17) 0.0793(13) 0.061(8) Uiso 0.151(8) d PD A 2 F5' F 0.7966(11) 0.2234(19) 0.0587(13) 0.047(7) Uiso 0.151(8) d PD A 2 F6 F 0.9095(3) 0.1589(3) 0.0734(2) 0.0875(14) Uani 1 d D . . N1S N 0.1419(3) 0.1030(4) 0.1810(3) 0.0553(13) Uani 1 d . . . C1S C 0.1133(3) 0.0960(5) 0.0204(3) 0.0436(13) Uani 1 d . . . H1S1 H 0.0645 0.1438 -0.0002 0.065 Uiso 1 calc R . . H1S2 H 0.1002 0.0206 0.0015 0.065 Uiso 1 calc R . . H1S3 H 0.1646 0.1218 -0.0011 0.065 Uiso 1 calc R . . C2S C 0.1287(3) 0.0986(4) 0.1101(4) 0.0382(12) Uani 1 d . . . 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 0.0196(3) 0.0283(3) 0.0164(2) 0.0018(2) 0.00442(19) 0.0010(2) Zn2 0.0195(3) 0.0292(3) 0.0183(3) 0.0005(2) 0.00468(19) -0.0010(2) O1 0.0171(15) 0.0330(17) 0.0170(15) -0.0017(12) 0.0015(12) -0.0013(13) O2 0.0208(15) 0.0310(17) 0.0182(15) 0.0035(13) 0.0037(12) 0.0030(13) N1 0.0229(19) 0.030(2) 0.0240(19) 0.0015(16) 0.0082(16) 0.0003(16) N2 0.029(2) 0.032(2) 0.0171(18) 0.0009(16) 0.0077(15) 0.0022(17) N3 0.0220(19) 0.034(2) 0.0218(19) -0.0006(16) 0.0079(15) -0.0031(16) N4 0.0213(19) 0.028(2) 0.0248(19) -0.0022(16) 0.0060(16) 0.0007(16) C1 0.025(2) 0.022(2) 0.022(2) 0.0001(18) 0.0033(18) -0.0001(18) C2 0.022(2) 0.020(2) 0.023(2) 0.0001(18) 0.0019(18) -0.0003(18) C3 0.022(2) 0.019(2) 0.034(3) -0.0012(19) 0.0051(19) -0.0034(18) C4 0.026(2) 0.022(2) 0.024(2) 0.0004(18) -0.0055(19) -0.0012(18) C5 0.031(2) 0.028(2) 0.018(2) -0.0009(18) 0.0006(18) 0.0012(19) C6 0.023(2) 0.023(2) 0.022(2) -0.0018(18) 0.0040(18) -0.0001(18) C7 0.031(3) 0.028(2) 0.030(3) 0.001(2) -0.006(2) 0.000(2) C8 0.020(2) 0.023(2) 0.031(2) 0.0040(19) 0.0088(19) 0.0003(18) C9 0.026(2) 0.049(3) 0.029(2) 0.005(2) 0.012(2) 0.000(2) C10 0.034(3) 0.041(3) 0.023(2) 0.002(2) 0.012(2) 0.012(2) C11 0.035(3) 0.051(3) 0.022(2) -0.003(2) 0.012(2) 0.007(2) C12 0.035(2) 0.024(2) 0.016(2) 0.0048(18) 0.0043(18) 0.003(2) C13 0.026(2) 0.022(2) 0.022(2) 0.0028(18) 0.0016(18) -0.0027(18) C14 0.034(3) 0.027(2) 0.022(2) 0.0015(19) -0.0028(19) 0.001(2) C15 0.032(3) 0.028(3) 0.032(3) 0.000(2) -0.006(2) -0.002(2) C16 0.025(2) 0.031(3) 0.037(3) -0.002(2) 0.001(2) 0.003(2) C17 0.021(2) 0.024(2) 0.028(2) -0.0005(18) 0.0019(18) 0.0018(18) C18 0.022(2) 0.020(2) 0.024(2) 0.0037(17) 0.0006(18) 0.0002(17) C19 0.039(3) 0.053(3) 0.038(3) 0.001(3) -0.012(2) 0.008(3) C20 0.019(2) 0.024(2) 0.037(3) -0.002(2) 0.0024(19) 0.0006(18) C21 0.027(2) 0.046(3) 0.029(3) 0.000(2) 0.015(2) 0.001(2) C22 0.034(3) 0.043(3) 0.029(3) -0.007(2) 0.018(2) -0.002(2) C23 0.026(2) 0.052(3) 0.026(2) 0.001(2) 0.011(2) -0.007(2) C24 0.028(2) 0.029(2) 0.015(2) 0.0015(18) 0.0010(18) 0.0017(19) C25 0.025(2) 0.031(2) 0.019(2) 0.0014(19) -0.0023(18) -0.001(2) C26 0.031(3) 0.028(3) 0.036(3) 0.003(2) 0.001(2) -0.001(2) O3 0.0262(16) 0.0282(16) 0.0249(16) 0.0028(13) 0.0057(13) 0.0010(13) O4 0.0265(16) 0.0285(17) 0.0312(17) 0.0011(14) 0.0065(13) -0.0015(14) P 0.0296(6) 0.0352(7) 0.0319(6) -0.0027(6) -0.0001(5) -0.0016(6) F1 0.124(4) 0.061(3) 0.082(3) 0.026(2) -0.028(3) 0.009(3) F2 0.066(4) 0.096(5) 0.207(8) -0.015(5) -0.023(4) -0.041(3) F3 0.132(5) 0.110(5) 0.030(2) -0.020(3) 0.008(3) 0.045(4) F4 0.042(3) 0.128(5) 0.151(6) -0.023(4) -0.001(3) -0.045(3) F5 0.101(4) 0.107(5) 0.075(3) -0.007(3) 0.039(3) 0.055(4) F6 0.154(4) 0.065(3) 0.037(2) 0.0028(18) -0.005(2) 0.033(3) N1S 0.064(3) 0.057(3) 0.047(3) 0.005(3) 0.017(3) 0.007(3) C1S 0.037(3) 0.050(3) 0.044(3) -0.005(3) 0.006(2) -0.002(3) C2S 0.038(3) 0.034(3) 0.045(3) 0.005(2) 0.014(2) 0.004(2) _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 2.030(4) . y Zn1 N2 2.056(3) . y Zn1 O2 2.036(3) . y Zn1 O3 2.011(3) . y Zn1 O1 2.074(3) . y Zn2 N3 2.039(4) . y Zn2 N4 2.054(4) . y Zn2 O1 2.055(3) . y Zn2 O2 2.079(3) . y Zn2 O4 2.007(3) . y Zn1 Zn2 3.0376(10) . y O1 C1 1.311(5) . ? O2 C18 1.315(5) . ? N1 C8 1.287(6) . ? N1 C9 1.475(5) . ? N2 C12 1.280(5) . ? N2 C11 1.484(5) . ? N3 C24 1.280(5) . ? N3 C23 1.468(5) . ? N4 C20 1.289(6) . ? N4 C21 1.489(5) . ? C1 C6 1.416(6) . ? C1 C2 1.422(6) . ? C2 C3 1.411(6) . ? C2 C8 1.450(6) . ? C3 C4 1.382(6) . ? C4 C5 1.383(6) . ? C4 C7 1.512(6) . ? C5 C6 1.404(6) . ? C6 C24 1.441(6) . ? C9 C10 1.520(7) . ? C10 C11 1.502(6) . ? C12 C13 1.450(6) . ? C13 C14 1.398(6) . ? C13 C18 1.422(6) . ? C14 C15 1.380(7) . ? C15 C16 1.381(7) . ? C15 C19 1.508(6) . ? C16 C17 1.409(6) . ? C17 C18 1.413(6) . ? C17 C20 1.446(6) . ? C21 C22 1.506(7) . ? C22 C23 1.522(7) . ? C25 O3 1.253(5) . ? C25 O4 1.267(5) . ? C25 C26 1.507(6) . ? P F1 1.564(4) . ? P F2 1.566(5) . ? P F3 1.575(4) . ? P F4 1.538(4) . ? P F5 1.562(4) . ? P F6 1.574(4) . ? P F2' 1.553(13) . ? P F3' 1.548(13) . ? P F4' 1.559(13) . ? P F5' 1.569(13) . ? N1S C2S 1.139(7) . ? C1S C2S 1.439(7) . ? 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 O3 Zn1 N1 110.07(13) . . y O3 Zn1 O2 100.36(12) . . y N1 Zn1 O2 146.81(14) . . y O3 Zn1 N2 101.55(13) . . y N1 Zn1 N2 97.06(14) . . y O2 Zn1 N2 89.35(13) . . y O3 Zn1 O1 94.99(12) . . y N1 Zn1 O1 87.60(13) . . y O2 Zn1 O1 76.61(11) . . y N2 Zn1 O1 160.02(13) . . y O3 Zn1 Zn2 79.33(8) . . ? N1 Zn1 Zn2 129.97(10) . . ? O2 Zn1 Zn2 42.97(8) . . ? N2 Zn1 Zn2 130.16(10) . . ? O1 Zn1 Zn2 42.40(8) . . ? O4 Zn2 N3 105.12(14) . . y O4 Zn2 N4 112.81(13) . . y N3 Zn2 N4 96.19(14) . . y O4 Zn2 O1 97.98(12) . . y N3 Zn2 O1 88.10(13) . . y N4 Zn2 O1 146.39(13) . . y O4 Zn2 O2 94.37(12) . . y N3 Zn2 O2 156.48(13) . . y N4 Zn2 O2 88.03(13) . . y O1 Zn2 O2 76.08(11) . . y O4 Zn2 Zn1 77.56(8) . . ? N3 Zn2 Zn1 129.65(10) . . ? N4 Zn2 Zn1 129.91(10) . . ? O1 Zn2 Zn1 42.87(8) . . ? O2 Zn2 Zn1 41.89(8) . . ? C1 O1 Zn2 130.2(3) . . ? C1 O1 Zn1 128.3(3) . . ? Zn2 O1 Zn1 94.73(11) . . y C18 O2 Zn1 130.0(3) . . ? C18 O2 Zn2 128.4(3) . . ? Zn1 O2 Zn2 95.14(12) . . y C8 N1 C9 116.8(4) . . ? C8 N1 Zn1 126.2(3) . . ? C9 N1 Zn1 116.7(3) . . ? C12 N2 C11 115.2(4) . . ? C12 N2 Zn1 125.0(3) . . ? C11 N2 Zn1 119.8(3) . . ? C24 N3 C23 116.8(4) . . ? C24 N3 Zn2 126.0(3) . . ? C23 N3 Zn2 117.2(3) . . ? C20 N4 C21 113.9(4) . . ? C20 N4 Zn2 124.5(3) . . ? C21 N4 Zn2 121.6(3) . . ? O1 C1 C6 121.4(4) . . ? O1 C1 C2 121.2(4) . . ? C6 C1 C2 117.4(4) . . ? C3 C2 C1 119.9(4) . . ? C3 C2 C8 115.9(4) . . ? C1 C2 C8 124.2(4) . . ? C4 C3 C2 122.7(4) . . ? C3 C4 C5 116.8(4) . . ? C3 C4 C7 122.5(4) . . ? C5 C4 C7 120.7(4) . . ? C4 C5 C6 123.3(4) . . ? C5 C6 C1 119.8(4) . . ? C5 C6 C24 115.8(4) . . ? C1 C6 C24 124.5(4) . . ? N1 C8 C2 127.6(4) . . ? N1 C9 C10 110.5(4) . . ? C11 C10 C9 114.9(4) . . ? N2 C11 C10 112.6(4) . . ? N2 C12 C13 128.3(4) . . ? C14 C13 C18 119.3(4) . . ? C14 C13 C12 116.0(4) . . ? C18 C13 C12 124.7(4) . . ? C15 C14 C13 123.6(4) . . ? C14 C15 C16 116.5(4) . . ? C14 C15 C19 121.5(4) . . ? C16 C15 C19 121.9(5) . . ? C15 C16 C17 123.0(4) . . ? C16 C17 C18 119.6(4) . . ? C16 C17 C20 115.6(4) . . ? C18 C17 C20 124.8(4) . . ? O2 C18 C17 120.4(4) . . ? O2 C18 C13 121.8(4) . . ? C17 C18 C13 117.8(4) . . ? N4 C20 C17 128.7(4) . . ? N4 C21 C22 114.0(4) . . ? C21 C22 C23 113.8(4) . . ? N3 C23 C22 110.0(4) . . ? N3 C24 C6 128.3(4) . . ? O3 C25 O4 125.9(4) . . ? O3 C25 C26 117.2(4) . . ? O4 C25 C26 116.9(4) . . ? C25 O3 Zn1 126.9(3) . . ? C25 O4 Zn2 129.2(3) . . ? F3' P F2' 90.2(13) . . ? F3' P F4' 93.8(14) . . ? F2' P F4' 173.6(12) . . ? F4 P F5 89.2(3) . . ? F4 P F1 92.6(3) . . ? F3' P F1 82.1(9) . . ? F2' P F1 91.6(8) . . ? F4' P F1 93.8(9) . . ? F5 P F1 86.7(3) . . ? F4 P F2 177.4(4) . . ? F5 P F2 92.0(4) . . ? F1 P F2 85.2(3) . . ? F3' P F5' 173.0(13) . . ? F2' P F5' 84.8(12) . . ? F4' P F5' 90.7(13) . . ? F1 P F5' 103.0(8) . . ? F4 P F6 88.5(3) . . ? F3' P F6 99.5(9) . . ? F2' P F6 88.2(8) . . ? F4' P F6 86.3(9) . . ? F5 P F6 92.3(2) . . ? F1 P F6 178.5(3) . . ? F2 P F6 93.7(3) . . ? F4 P F3 92.5(4) . . ? F5 P F3 177.8(4) . . ? F1 P F3 94.6(3) . . ? F2 P F3 86.3(4) . . ? F6 P F3 86.4(2) . . ? C1S C2S N1S 178.4(6) . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.67 _refine_diff_density_min -0.47 _refine_diff_density_rms 0.09 #===END data_6 _database_code_CSD 197072 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C26 H30 Cl2 N4 O2 Zn2' _chemical_formula_sum 'C26 H30 Cl2 N4 O2 Zn2' _chemical_formula_weight 632.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.352(4) _cell_length_b 17.660(9) _cell_length_c 9.967(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.74(2) _cell_angle_gamma 90.00 _cell_volume 1251.5(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 37 _cell_measurement_theta_min 15 _cell_measurement_theta_max 16 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.73 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.678 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 2.163 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.831 _exptl_absorpt_correction_T_max 0.948 _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 'Stoe Stadi-4 four-circle' _diffrn_measurement_method omega/2-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 1631 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_sigmaI/netI 0.015 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 22.49 _reflns_number_total 1631 _reflns_number_gt 1480 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DIF4 (Stoe & Cie, 1992a)' _computing_cell_refinement 'DIF4 (Stoe & Cie, 1992a)' _computing_data_reduction 'REDU4 (Stoe & Cie, 1992b)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELTXL/PC (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2002)' _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 w=1/[\s^2^(Fo^2^)+(0.024P)^2^+1.73P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1631 _refine_ls_number_parameters 166 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0255 _refine_ls_R_factor_gt 0.0216 _refine_ls_wR_factor_ref 0.0563 _refine_ls_wR_factor_gt 0.0538 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.97566(4) 0.498210(16) 0.15647(3) 0.01781(12) Uani 1 d . . . Cl Cl 1.17643(9) 0.55336(4) 0.33737(7) 0.02487(18) Uani 1 d . . . O1 O 1.0773(3) 0.43750(10) 0.02328(18) 0.0223(4) Uani 1 d . . . N1 N 0.8747(3) 0.39565(12) 0.2094(2) 0.0211(5) Uani 1 d . . . N2 N 0.7127(3) 0.53691(12) 0.1609(2) 0.0198(5) Uani 1 d . . . C1 C 1.1258(4) 0.36568(14) 0.0247(3) 0.0190(6) Uani 1 d . . . C2 C 1.0455(4) 0.30961(14) 0.0956(3) 0.0184(6) Uani 1 d . . . C3 C 1.0991(4) 0.23386(15) 0.0857(3) 0.0231(6) Uani 1 d . . . H3 H 1.0457 0.1962 0.1322 0.028 Uiso 1 calc R . . C4 C 1.2258(4) 0.21123(15) 0.0118(3) 0.0244(6) Uani 1 d . . . C5 C 1.3064(4) 0.26697(15) -0.0524(3) 0.0235(6) Uani 1 d . . . H5 H 1.3960 0.2524 -0.1014 0.028 Uiso 1 calc R . . C6 C 1.2613(4) 0.34363(15) -0.0479(3) 0.0199(6) Uani 1 d . . . C7 C 1.2751(4) 0.12886(16) -0.0009(3) 0.0320(7) Uani 1 d . . . H7A H 1.4084 0.1208 0.0446 0.038 Uiso 1 calc R . . H7B H 1.2509 0.1152 -0.0992 0.038 Uiso 1 calc R . . H7C H 1.1979 0.0971 0.0436 0.038 Uiso 1 calc R . . C8 C 0.9044(4) 0.32719(15) 0.1765(3) 0.0207(6) Uani 1 d . . . C9 C 0.7998(4) 0.26100(16) 0.2161(3) 0.0305(7) Uani 1 d . . . H9A H 0.8780 0.2368 0.2995 0.037 Uiso 1 calc R . . H9B H 0.7711 0.2243 0.1399 0.037 Uiso 1 calc R . . H9C H 0.6825 0.2788 0.2349 0.037 Uiso 1 calc R . . C10 C 0.7441(4) 0.41759(16) 0.2933(3) 0.0305(7) Uani 1 d . . . H10A H 0.8168 0.4362 0.3850 0.037 Uiso 1 calc R . . H10B H 0.6710 0.3728 0.3085 0.037 Uiso 1 calc R . . C11 C 0.6093(4) 0.47959(16) 0.2204(3) 0.0280(7) Uani 1 d . . . H11A H 0.5090 0.4569 0.1456 0.034 Uiso 1 calc R . . H11B H 0.5494 0.5040 0.2877 0.034 Uiso 1 calc R . . C12 C 1.3620(4) 0.39971(15) -0.1143(3) 0.0213(6) Uani 1 d . . . C13 C 1.5592(4) 0.38068(18) -0.1216(3) 0.0306(7) Uani 1 d . . . H13A H 1.5578 0.3655 -0.2165 0.037 Uiso 1 calc R . . H13B H 1.6080 0.3389 -0.0578 0.037 Uiso 1 calc R . . H13C H 1.6400 0.4252 -0.0954 0.037 Uiso 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 0.0219(2) 0.01460(19) 0.01933(19) -0.00051(12) 0.00972(14) -0.00086(12) Cl 0.0274(4) 0.0226(4) 0.0249(4) -0.0035(3) 0.0072(3) -0.0051(3) O1 0.0349(11) 0.0144(10) 0.0226(10) 0.0014(8) 0.0163(8) 0.0046(8) N1 0.0275(13) 0.0182(13) 0.0204(12) -0.0008(10) 0.0113(10) -0.0034(10) N2 0.0210(12) 0.0205(13) 0.0205(12) -0.0035(10) 0.0102(10) -0.0038(10) C1 0.0215(14) 0.0179(14) 0.0151(13) -0.0016(11) 0.0002(11) 0.0014(12) C2 0.0210(14) 0.0167(14) 0.0159(14) -0.0002(11) 0.0017(11) -0.0013(11) C3 0.0266(15) 0.0176(15) 0.0227(15) 0.0016(12) 0.0023(12) -0.0008(12) C4 0.0282(16) 0.0211(15) 0.0201(14) -0.0016(12) -0.0011(12) 0.0048(12) C5 0.0222(15) 0.0264(16) 0.0198(14) -0.0054(12) 0.0016(12) 0.0053(12) C6 0.0213(14) 0.0189(14) 0.0174(14) -0.0007(11) 0.0014(11) 0.0031(11) C7 0.0368(18) 0.0222(16) 0.0343(17) 0.0000(13) 0.0042(14) 0.0088(13) C8 0.0228(15) 0.0201(15) 0.0171(14) 0.0018(11) 0.0013(12) -0.0024(12) C9 0.0351(17) 0.0195(15) 0.0401(18) 0.0024(13) 0.0157(14) -0.0028(13) C10 0.0402(18) 0.0268(16) 0.0307(17) 0.0002(13) 0.0203(14) -0.0060(14) C11 0.0290(16) 0.0286(16) 0.0300(16) -0.0061(13) 0.0144(13) -0.0051(13) C12 0.0217(14) 0.0249(16) 0.0169(14) -0.0062(12) 0.0042(11) 0.0020(12) C13 0.0269(16) 0.0356(17) 0.0318(16) 0.0009(14) 0.0121(13) 0.0081(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.994(2) . y Zn1 N2 2.062(2) . y Zn1 O1 2.072(2) 3_765 y Zn1 N1 2.076(2) . y Zn1 Cl 2.2414(11) . y Zn1 Zn1 3.229(2) 3_765 y O1 C1 1.317(3) . ? O1 Zn1 2.072(2) 3_765 y N1 C8 1.286(3) . ? N1 C10 1.476(4) . ? N2 C12 1.281(4) 3_765 ? N2 C11 1.477(4) . ? C1 C6 1.427(4) . ? C1 C2 1.428(4) . ? C2 C3 1.405(4) . ? C2 C8 1.500(4) . ? C3 C4 1.386(4) . ? C4 C5 1.386(4) . ? C4 C7 1.512(4) . ? C5 C6 1.397(4) . ? C6 C12 1.488(4) . ? C8 C9 1.506(4) . ? C10 C11 1.531(4) . ? C12 N2 1.281(4) 3_765 ? C12 C13 1.508(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 N2 134.84(8) . . y O1 Zn1 O1 74.86(9) . 3_765 y N2 Zn1 O1 82.30(8) . 3_765 y O1 Zn1 N1 85.35(8) . . y N2 Zn1 N1 83.45(9) . . y O1 Zn1 N1 134.19(8) 3_765 . y O1 Zn1 Cl 119.18(7) . . y N2 Zn1 Cl 105.54(7) . . y O1 Zn1 Cl 113.44(6) 3_765 . y N1 Zn1 Cl 112.30(7) . . y O1 Zn1 Zn1 38.28(5) . 3_765 ? N2 Zn1 Zn1 110.45(6) . 3_765 ? O1 Zn1 Zn1 36.58(5) 3_765 3_765 ? N1 Zn1 Zn1 113.41(6) . 3_765 ? Cl Zn1 Zn1 123.80(4) . 3_765 ? C1 O1 Zn1 131.08(16) . . ? C1 O1 Zn1 121.87(16) . 3_765 ? Zn1 O1 Zn1 105.14(9) . 3_765 y C8 N1 C10 124.6(2) . . ? C8 N1 Zn1 131.37(19) . . ? C10 N1 Zn1 103.95(16) . . ? C12 N2 C11 121.9(2) 3_765 . ? C12 N2 Zn1 126.82(18) 3_765 . ? C11 N2 Zn1 111.26(17) . . ? O1 C1 C6 118.7(2) . . ? O1 C1 C2 121.9(2) . . ? C6 C1 C2 119.4(2) . . ? C3 C2 C1 117.8(2) . . ? C3 C2 C8 118.6(2) . . ? C1 C2 C8 123.5(2) . . ? C4 C3 C2 123.4(3) . . ? C3 C4 C5 117.7(2) . . ? C3 C4 C7 122.0(3) . . ? C5 C4 C7 120.3(3) . . ? C4 C5 C6 122.7(3) . . ? C5 C6 C1 118.8(2) . . ? C5 C6 C12 118.8(2) . . ? C1 C6 C12 122.3(2) . . ? N1 C8 C2 121.1(2) . . ? N1 C8 C9 122.1(2) . . ? C2 C8 C9 116.7(2) . . ? N1 C10 C11 110.8(2) . . ? N2 C11 C10 110.1(2) . . ? N2 C12 C6 121.8(2) 3_765 . ? N2 C12 C13 120.4(3) 3_765 . ? C6 C12 C13 117.8(2) . . ? 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 N2 Zn1 O1 C1 -101.7(2) . . . . ? O1 Zn1 O1 C1 -164.0(3) 3_765 . . . ? N1 Zn1 O1 C1 -25.8(2) . . . . ? Cl Zn1 O1 C1 87.2(2) . . . . ? Zn1 Zn1 O1 C1 -164.0(3) 3_765 . . . ? N2 Zn1 O1 Zn1 62.31(13) . . . 3_765 ? O1 Zn1 O1 Zn1 0.0 3_765 . . 3_765 ? N1 Zn1 O1 Zn1 138.29(10) . . . 3_765 ? Cl Zn1 O1 Zn1 -108.72(7) . . . 3_765 ? O1 Zn1 N1 C8 9.2(2) . . . . ? N2 Zn1 N1 C8 145.4(2) . . . . ? O1 Zn1 N1 C8 72.8(3) 3_765 . . . ? Cl Zn1 N1 C8 -110.5(2) . . . . ? Zn1 Zn1 N1 C8 35.9(3) 3_765 . . . ? O1 Zn1 N1 C10 -167.87(17) . . . . ? N2 Zn1 N1 C10 -31.70(17) . . . . ? O1 Zn1 N1 C10 -104.27(18) 3_765 . . . ? Cl Zn1 N1 C10 72.43(17) . . . . ? Zn1 Zn1 N1 C10 -141.18(15) 3_765 . . . ? O1 Zn1 N2 C12 -90.4(2) . . . 3_765 ? O1 Zn1 N2 C12 -30.8(2) 3_765 . . 3_765 ? N1 Zn1 N2 C12 -167.2(2) . . . 3_765 ? Cl Zn1 N2 C12 81.5(2) . . . 3_765 ? Zn1 Zn1 N2 C12 -54.6(2) 3_765 . . 3_765 ? O1 Zn1 N2 C11 86.65(19) . . . . ? O1 Zn1 N2 C11 146.25(18) 3_765 . . . ? N1 Zn1 N2 C11 9.90(17) . . . . ? Cl Zn1 N2 C11 -101.48(17) . . . . ? Zn1 Zn1 N2 C11 122.48(16) 3_765 . . . ? Zn1 O1 C1 C6 -154.71(18) . . . . ? Zn1 O1 C1 C6 43.5(3) 3_765 . . . ? Zn1 O1 C1 C2 25.9(4) . . . . ? Zn1 O1 C1 C2 -135.9(2) 3_765 . . . ? O1 C1 C2 C3 177.0(2) . . . . ? C6 C1 C2 C3 -2.4(4) . . . . ? O1 C1 C2 C8 -1.6(4) . . . . ? C6 C1 C2 C8 179.1(2) . . . . ? C1 C2 C3 C4 0.3(4) . . . . ? C8 C2 C3 C4 178.9(2) . . . . ? C2 C3 C4 C5 1.7(4) . . . . ? C2 C3 C4 C7 -177.8(2) . . . . ? C3 C4 C5 C6 -1.6(4) . . . . ? C7 C4 C5 C6 177.8(2) . . . . ? C4 C5 C6 C1 -0.4(4) . . . . ? C4 C5 C6 C12 177.1(2) . . . . ? O1 C1 C6 C5 -176.9(2) . . . . ? C2 C1 C6 C5 2.5(4) . . . . ? O1 C1 C6 C12 5.6(4) . . . . ? C2 C1 C6 C12 -175.0(2) . . . . ? C10 N1 C8 C2 -177.5(2) . . . . ? Zn1 N1 C8 C2 5.9(4) . . . . ? C10 N1 C8 C9 2.8(4) . . . . ? Zn1 N1 C8 C9 -173.77(19) . . . . ? C3 C2 C8 N1 167.7(2) . . . . ? C1 C2 C8 N1 -13.8(4) . . . . ? C3 C2 C8 C9 -12.6(3) . . . . ? C1 C2 C8 C9 165.9(2) . . . . ? C8 N1 C10 C11 -128.7(3) . . . . ? Zn1 N1 C10 C11 48.6(2) . . . . ? C12 N2 C11 C10 -168.7(2) 3_765 . . . ? Zn1 N2 C11 C10 14.1(3) . . . . ? N1 C10 C11 N2 -42.8(3) . . . . ? C5 C6 C12 N2 153.2(2) . . . 3_765 ? C1 C6 C12 N2 -29.4(4) . . . 3_765 ? C5 C6 C12 C13 -28.6(3) . . . . ? C1 C6 C12 C13 148.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.28 _refine_diff_density_min -0.23 _refine_diff_density_rms 0.05 #===END data_3 _database_code_CSD 199496 # Code ZNONC4 #330 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C30 H36 N4 O6 Zn2, C H Cl3' _chemical_formula_sum 'C31 H37 Cl3 N4 O6 Zn2' _chemical_formula_weight 798.74 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.565(7) _cell_length_b 12.732(3) _cell_length_c 13.289(2) _cell_angle_alpha 112.75(3) _cell_angle_beta 96.16(3) _cell_angle_gamma 108.63(3) _cell_volume 1649.2(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 41 _cell_measurement_theta_min 16 _cell_measurement_theta_max 18.15 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 820 _exptl_absorpt_coefficient_mu 1.747 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.453 _exptl_absorpt_correction_T_max 0.559 _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 'Stoe Stadi-4 four circle' _diffrn_measurement_method Omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 13 _diffrn_reflns_number 5093 _diffrn_reflns_av_R_equivalents 0.099 _diffrn_reflns_av_sigmaI/netI 0.057 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4650 _reflns_number_gt 3524 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stadi-4 (Stoe & Cie, 1995a)' _computing_cell_refinement 'Stadi-4 (Stoe & Cie, 1995a)' _computing_data_reduction 'X-red (Stoe & Cie, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2002)' _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^)+(0.054P)^2^+21.64P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4650 _refine_ls_number_parameters 419 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0933 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.187 _refine_ls_wR_factor_gt 0.163 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0.003 _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 0.30024(10) 0.11312(10) -0.32574(9) 0.0192(3) Uani 1 1 d . . . Zn2 Zn 0.33385(9) 0.23364(10) -0.06492(9) 0.0199(3) Uani 1 1 d . . . O1 O 0.2818(5) 0.2664(6) -0.2024(5) 0.0190(14) Uani 1 1 d . . . O2 O 0.4280(5) 0.1634(6) -0.1712(5) 0.0223(14) Uani 1 1 d . . . O3 O 0.2884(6) -0.0574(6) -0.4315(5) 0.0280(16) Uani 1 1 d . . . O4 O 0.2375(7) -0.2587(6) -0.5006(6) 0.0329(17) Uani 1 1 d . . . O5 O 0.1432(6) 0.0059(6) -0.2725(5) 0.0257(15) Uani 1 1 d . . . O6 O 0.1769(6) 0.1000(6) -0.0841(5) 0.0258(15) Uani 1 1 d . . . N1 N 0.1751(7) 0.1260(7) -0.4418(6) 0.0192(17) Uani 1 1 d . . . N2 N 0.4697(7) 0.1959(7) -0.3621(6) 0.0221(18) Uani 1 1 d . . . N3 N 0.3577(7) 0.4110(7) 0.0310(6) 0.0222(18) Uani 1 1 d . . . N4 N 0.4450(7) 0.2145(7) 0.0591(6) 0.0197(17) Uani 1 1 d . . . C1 C 0.1977(8) 0.3149(9) -0.2040(8) 0.022(2) Uani 1 1 d . . . C2 C 0.1045(9) 0.2731(9) -0.3054(8) 0.022(2) Uani 1 1 d . . . C3 C 0.0156(8) 0.3286(9) -0.3024(8) 0.022(2) Uani 1 1 d . . . H3 H -0.0482 0.2983 -0.3697 0.026 Uiso 1 1 calc R . . C4 C 0.0178(9) 0.4242(9) -0.2065(8) 0.026(2) Uani 1 1 d . . . C5 C 0.1135(9) 0.4687(9) -0.1103(8) 0.024(2) Uani 1 1 d . . . H5 H 0.1206 0.5388 -0.0445 0.029 Uiso 1 1 calc R . . C6 C 0.1997(8) 0.4141(8) -0.1068(7) 0.018(2) Uani 1 1 d . . . C7 C -0.0759(10) 0.4843(10) -0.2080(9) 0.036(3) Uani 1 1 d . . . H7A H -0.0336 0.5646 -0.2077 0.054 Uiso 1 1 calc R . . H7B H -0.1083 0.4966 -0.1410 0.054 Uiso 1 1 calc R . . H7C H -0.1462 0.4306 -0.2764 0.054 Uiso 1 1 calc R . . C8 C 0.1005(9) 0.1831(8) -0.4162(8) 0.024(2) Uani 1 1 d . . . H8 H 0.0344 0.1642 -0.4774 0.029 Uiso 1 1 calc R . . C9 C 0.1538(9) 0.0471(9) -0.5630(7) 0.024(2) Uani 1 1 d . . . H9A H 0.0684 0.0299 -0.6046 0.029 Uiso 1 1 calc R . . H9B H 0.1573 -0.0330 -0.5733 0.029 Uiso 1 1 calc R . . C10 C 0.2521(9) 0.1085(10) -0.6119(8) 0.028(2) Uani 1 1 d . . . H10A H 0.2515 0.1910 -0.5958 0.034 Uiso 1 1 calc R . . H10B H 0.2256 0.0586 -0.6951 0.034 Uiso 1 1 calc R . . C11 C 0.3883(9) 0.1258(10) -0.5690(8) 0.033(3) Uani 1 1 d . . . H11A H 0.3864 0.0488 -0.5660 0.040 Uiso 1 1 calc R . . H11B H 0.4348 0.1363 -0.6252 0.040 Uiso 1 1 calc R . . C12 C 0.4627(9) 0.2341(9) -0.4537(8) 0.028(2) Uani 1 1 d . . . H12A H 0.5496 0.2759 -0.4569 0.034 Uiso 1 1 calc R . . H12B H 0.4224 0.2947 -0.4359 0.034 Uiso 1 1 calc R . . C13 C 0.5801(8) 0.2019(8) -0.3228(7) 0.022(2) Uani 1 1 d . . . H13 H 0.6422 0.2203 -0.3617 0.026 Uiso 1 1 calc R . . C14 C 0.6188(8) 0.1836(8) -0.2255(8) 0.020(2) Uani 1 1 d . . . C15 C 0.7413(8) 0.1853(9) -0.2016(8) 0.024(2) Uani 1 1 d . . . H15 H 0.7900 0.1896 -0.2541 0.029 Uiso 1 1 calc R . . C16 C 0.7942(8) 0.1809(9) -0.1060(8) 0.026(2) Uani 1 1 d . . . C17 C 0.7249(9) 0.1808(9) -0.0282(8) 0.026(2) Uani 1 1 d . . . H17 H 0.7615 0.1813 0.0396 0.031 Uiso 1 1 calc R . . C18 C 0.6027(8) 0.1801(9) -0.0443(7) 0.021(2) Uani 1 1 d . . . C19 C 0.5446(8) 0.1739(8) -0.1488(8) 0.019(2) Uani 1 1 d . . . C20 C 0.9251(9) 0.1810(11) -0.0840(9) 0.037(3) Uani 1 1 d . . . H20A H 0.9493 0.1545 -0.1554 0.055 Uiso 1 1 calc R . . H20B H 0.9255 0.1239 -0.0515 0.055 Uiso 1 1 calc R . . H20C H 0.9857 0.2648 -0.0310 0.055 Uiso 1 1 calc R . . C21 C 0.5435(8) 0.1916(9) 0.0475(8) 0.023(2) Uani 1 1 d . . . H21 H 0.5831 0.1806 0.1070 0.027 Uiso 1 1 calc R . . C22 C 0.4007(10) 0.2214(10) 0.1603(9) 0.035(3) Uani 1 1 d . . . H22A H 0.4750 0.2564 0.2254 0.042 Uiso 1 1 calc R . . H22B H 0.3488 0.1365 0.1478 0.042 Uiso 1 1 calc R . . C23 C 0.3239(9) 0.2991(10) 0.1892(8) 0.031(2) Uani 1 1 d . . . H23A H 0.2868 0.2878 0.2499 0.038 Uiso 1 1 calc R . . H23B H 0.2527 0.2650 0.1218 0.038 Uiso 1 1 calc R . . C24 C 0.3899(9) 0.4392(9) 0.2276(8) 0.025(2) Uani 1 1 d . . . H24A H 0.3272 0.4765 0.2463 0.030 Uiso 1 1 calc R . . H24B H 0.4571 0.4749 0.2982 0.030 Uiso 1 1 calc R . . C25 C 0.4490(8) 0.4789(9) 0.1443(8) 0.027(2) Uani 1 1 d . . . H25A H 0.4734 0.5692 0.1714 0.032 Uiso 1 1 calc R . . H25B H 0.5263 0.4616 0.1392 0.032 Uiso 1 1 calc R . . C26 C 0.2942(8) 0.4673(8) 0.0024(8) 0.021(2) Uani 1 1 d . . . H26 H 0.3097 0.5492 0.0557 0.025 Uiso 1 1 calc R . . C27 C 0.2793(8) -0.1526(10) -0.4197(8) 0.024(2) Uani 1 1 d . . . C28 C 0.3161(11) -0.1426(10) -0.3025(8) 0.039(3) Uani 1 1 d . . . H28A H 0.2399 -0.1799 -0.2821 0.058 Uiso 1 1 calc R . . H28B H 0.3603 -0.0551 -0.2479 0.058 Uiso 1 1 calc R . . H28C H 0.3721 -0.1862 -0.3018 0.058 Uiso 1 1 calc R . . C29 C 0.1176(9) 0.0113(9) -0.1818(9) 0.026(2) Uani 1 1 d . . . C30 C 0.0146(9) -0.1001(9) -0.1862(9) 0.031(2) Uani 1 1 d . . . H30A H -0.0539 -0.1371 -0.2551 0.047 Uiso 1 1 calc R . . H30B H -0.0184 -0.0743 -0.1198 0.047 Uiso 1 1 calc R . . H30C H 0.0492 -0.1611 -0.1865 0.047 Uiso 1 1 calc R . . C1S C 0.2197(11) 0.5195(10) -0.4589(9) 0.040(3) Uani 1 1 d . . . H1S H 0.2157 0.5920 -0.4696 0.047 Uiso 1 1 calc R . . Cl1 Cl 0.0821(3) 0.3912(3) -0.5423(3) 0.0672(11) Uani 1 1 d . . . Cl2 Cl 0.3532(3) 0.4935(3) -0.4987(3) 0.0592(9) Uani 1 1 d . . . Cl3 Cl 0.2399(3) 0.5556(3) -0.3147(2) 0.0527(9) Uani 1 1 d . . . 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 0.0197(5) 0.0256(6) 0.0144(6) 0.0082(5) 0.0021(4) 0.0133(5) Zn2 0.0181(5) 0.0280(6) 0.0147(6) 0.0086(5) 0.0023(4) 0.0120(5) O1 0.021(3) 0.026(4) 0.014(3) 0.007(3) 0.001(3) 0.016(3) O2 0.019(3) 0.039(4) 0.011(3) 0.010(3) 0.003(3) 0.015(3) O3 0.044(4) 0.021(4) 0.020(4) 0.007(3) 0.005(3) 0.018(3) O4 0.038(4) 0.032(4) 0.026(4) 0.013(4) 0.000(3) 0.015(3) O5 0.018(3) 0.032(4) 0.025(4) 0.013(3) 0.002(3) 0.009(3) O6 0.024(3) 0.029(4) 0.017(4) 0.006(3) 0.002(3) 0.007(3) N1 0.022(4) 0.026(4) 0.013(4) 0.011(4) 0.005(3) 0.012(4) N2 0.018(4) 0.034(5) 0.014(4) 0.011(4) 0.001(3) 0.011(4) N3 0.020(4) 0.022(4) 0.019(4) 0.007(4) 0.005(3) 0.005(4) N4 0.018(4) 0.027(4) 0.014(4) 0.008(4) 0.003(3) 0.011(3) C1 0.017(4) 0.033(6) 0.023(5) 0.018(5) 0.007(4) 0.010(4) C2 0.025(5) 0.033(6) 0.020(5) 0.016(5) 0.010(4) 0.018(4) C3 0.019(5) 0.028(5) 0.022(5) 0.012(5) 0.003(4) 0.012(4) C4 0.030(5) 0.038(6) 0.023(5) 0.019(5) 0.010(4) 0.023(5) C5 0.032(5) 0.023(5) 0.022(5) 0.007(4) 0.010(4) 0.020(5) C6 0.019(4) 0.018(5) 0.017(5) 0.008(4) -0.001(4) 0.007(4) C7 0.040(6) 0.047(7) 0.026(6) 0.010(5) 0.007(5) 0.033(6) C8 0.022(5) 0.023(5) 0.019(5) 0.010(4) -0.004(4) 0.003(4) C9 0.026(5) 0.031(6) 0.016(5) 0.010(5) 0.003(4) 0.013(5) C10 0.028(5) 0.043(6) 0.010(5) 0.008(5) 0.004(4) 0.016(5) C11 0.025(5) 0.050(7) 0.022(6) 0.014(5) 0.006(4) 0.014(5) C12 0.023(5) 0.036(6) 0.032(6) 0.020(5) 0.002(4) 0.015(5) C13 0.021(5) 0.022(5) 0.016(5) 0.004(4) 0.004(4) 0.006(4) C14 0.017(4) 0.024(5) 0.020(5) 0.007(4) 0.003(4) 0.013(4) C15 0.017(5) 0.028(6) 0.024(5) 0.006(4) 0.010(4) 0.012(4) C16 0.017(5) 0.028(6) 0.036(6) 0.014(5) 0.004(4) 0.013(4) C17 0.025(5) 0.033(6) 0.019(5) 0.009(5) 0.002(4) 0.016(5) C18 0.018(4) 0.027(5) 0.018(5) 0.007(4) 0.001(4) 0.012(4) C19 0.013(4) 0.014(5) 0.024(5) 0.003(4) 0.001(4) 0.006(4) C20 0.029(6) 0.050(7) 0.038(6) 0.019(6) 0.015(5) 0.021(5) C21 0.024(5) 0.030(5) 0.017(5) 0.011(4) 0.000(4) 0.014(4) C22 0.041(6) 0.040(7) 0.027(6) 0.016(5) 0.012(5) 0.018(5) C23 0.031(5) 0.047(7) 0.020(5) 0.017(5) 0.012(4) 0.016(5) C24 0.033(5) 0.032(6) 0.016(5) 0.009(4) 0.000(4) 0.022(5) C25 0.017(5) 0.033(6) 0.017(5) 0.003(5) -0.002(4) 0.005(4) C26 0.024(5) 0.016(5) 0.022(5) 0.006(4) 0.005(4) 0.010(4) C27 0.020(5) 0.036(7) 0.021(6) 0.014(5) 0.002(4) 0.015(5) C28 0.060(7) 0.037(7) 0.024(6) 0.012(5) 0.001(5) 0.029(6) C29 0.022(5) 0.037(6) 0.032(6) 0.021(6) 0.006(5) 0.021(5) C30 0.030(5) 0.033(6) 0.030(6) 0.014(5) 0.005(4) 0.011(5) C1S 0.049(7) 0.035(6) 0.036(7) 0.017(5) 0.012(5) 0.016(6) Cl1 0.070(2) 0.0457(19) 0.061(2) 0.0263(17) -0.0186(18) 0.0013(17) Cl2 0.077(2) 0.075(2) 0.056(2) 0.0395(19) 0.0334(18) 0.049(2) Cl3 0.074(2) 0.0389(17) 0.0340(17) 0.0164(14) 0.0179(15) 0.0068(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 Zn1 N1 2.090(7) . ? Zn1 N2 2.112(8) . ? Zn1 O1 2.099(6) . ? Zn1 O2 2.131(6) . ? Zn1 O3 2.028(6) . ? Zn2 N3 2.025(8) . ? Zn2 N4 2.117(7) . ? Zn2 O1 2.094(6) . ? Zn2 O2 1.988(6) . ? Zn1 O5 2.259(6) . ? Zn2 O6 1.961(6) . ? Zn1 Zn2 3.120(2) . ? O1 C1 1.311(11) . ? O2 C19 1.302(10) . ? O3 C27 1.256(12) . ? O4 C27 1.249(12) . ? O5 C29 1.254(11) . ? O6 C29 1.269(12) . ? N1 C8 1.288(12) . ? N1 C9 1.473(11) . ? N2 C13 1.293(11) . ? N2 C12 1.480(12) . ? N3 C26 1.300(12) . ? N3 C25 1.482(11) . ? N4 C21 1.274(11) . ? N4 C22 1.471(12) . ? C1 C6 1.406(13) . ? C1 C2 1.424(13) . ? C2 C3 1.417(12) . ? C2 C8 1.460(13) . ? C3 C4 1.371(13) . ? C4 C5 1.385(13) . ? C4 C7 1.516(13) . ? C5 C6 1.391(12) . ? C6 C26 1.478(12) . ? C9 C10 1.520(13) . ? C10 C11 1.531(13) . ? C11 C12 1.521(14) . ? C13 C14 1.450(13) . ? C14 C15 1.410(12) . ? C14 C19 1.417(13) . ? C15 C16 1.379(14) . ? C16 C17 1.374(13) . ? C16 C20 1.511(13) . ? C17 C18 1.403(12) . ? C18 C19 1.438(13) . ? C18 C21 1.443(13) . ? C22 C23 1.503(14) . ? C23 C24 1.539(14) . ? C24 C25 1.524(13) . ? C27 C28 1.513(13) . ? C29 C30 1.508(14) . ? C1S Cl1 1.729(12) . ? C1S Cl3 1.759(11) . ? C1S Cl2 1.772(12) . ? 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 O3 Zn1 N1 95.9(3) . . ? O3 Zn1 O1 166.7(3) . . ? N1 Zn1 O1 86.2(3) . . ? O3 Zn1 N2 90.2(3) . . ? N1 Zn1 N2 98.2(3) . . ? O1 Zn1 N2 102.5(3) . . ? O3 Zn1 O2 104.8(3) . . ? N1 Zn1 O2 159.4(3) . . ? O1 Zn1 O2 73.7(2) . . ? N2 Zn1 O2 82.3(3) . . ? O3 Zn1 O5 83.9(3) . . ? N1 Zn1 O5 93.3(3) . . ? O1 Zn1 O5 82.9(2) . . ? N2 Zn1 O5 167.6(3) . . ? O2 Zn1 O5 88.7(2) . . ? O3 Zn1 Zn2 129.97(19) . . ? N1 Zn1 Zn2 124.2(2) . . ? O1 Zn1 Zn2 41.87(16) . . ? N2 Zn1 Zn2 109.7(2) . . ? O2 Zn1 Zn2 39.08(16) . . ? O5 Zn1 Zn2 66.89(17) . . ? O6 Zn2 O2 109.2(3) . . ? O6 Zn2 N3 118.4(3) . . ? O2 Zn2 N3 131.3(3) . . ? O6 Zn2 O1 100.8(3) . . ? O2 Zn2 O1 76.8(2) . . ? N3 Zn2 O1 85.0(3) . . ? O6 Zn2 N4 95.0(3) . . ? O2 Zn2 N4 87.5(3) . . ? N3 Zn2 N4 97.3(3) . . ? O1 Zn2 N4 160.6(3) . . ? O6 Zn2 Zn1 90.17(19) . . ? O2 Zn2 Zn1 42.49(17) . . ? N3 Zn2 Zn1 125.2(2) . . ? O1 Zn2 Zn1 41.97(16) . . ? N4 Zn2 Zn1 127.7(2) . . ? C1 O1 Zn2 120.1(5) . . ? C1 O1 Zn1 131.5(6) . . ? Zn2 O1 Zn1 96.2(2) . . ? C19 O2 Zn2 128.6(6) . . ? C19 O2 Zn1 131.2(6) . . ? Zn2 O2 Zn1 98.4(2) . . ? C27 O3 Zn1 133.7(6) . . ? C29 O5 Zn1 137.3(6) . . ? C29 O6 Zn2 119.7(6) . . ? C8 N1 C9 116.3(7) . . ? C8 N1 Zn1 125.1(6) . . ? C9 N1 Zn1 117.8(6) . . ? C13 N2 C12 114.3(8) . . ? C13 N2 Zn1 126.2(6) . . ? C12 N2 Zn1 118.8(6) . . ? C26 N3 C25 117.7(8) . . ? C26 N3 Zn2 124.5(6) . . ? C25 N3 Zn2 117.7(6) . . ? C21 N4 C22 119.1(8) . . ? C21 N4 Zn2 123.3(6) . . ? C22 N4 Zn2 117.5(6) . . ? O1 C1 C6 121.3(8) . . ? O1 C1 C2 121.3(8) . . ? C6 C1 C2 117.4(8) . . ? C3 C2 C1 119.0(8) . . ? C3 C2 C8 116.7(8) . . ? C1 C2 C8 124.0(8) . . ? C4 C3 C2 122.8(9) . . ? C3 C4 C5 117.5(8) . . ? C3 C4 C7 121.1(9) . . ? C5 C4 C7 121.2(9) . . ? C4 C5 C6 122.1(9) . . ? C5 C6 C1 121.0(8) . . ? C5 C6 C26 116.9(8) . . ? C1 C6 C26 122.2(8) . . ? N1 C8 C2 128.5(8) . . ? N1 C9 C10 111.5(8) . . ? C9 C10 C11 116.7(8) . . ? C12 C11 C10 116.3(8) . . ? N2 C12 C11 112.9(8) . . ? N2 C13 C14 126.6(8) . . ? C15 C14 C19 118.4(8) . . ? C15 C14 C13 117.7(8) . . ? C19 C14 C13 123.7(8) . . ? C16 C15 C14 123.5(8) . . ? C17 C16 C15 117.5(8) . . ? C17 C16 C20 120.5(9) . . ? C15 C16 C20 122.0(9) . . ? C16 C17 C18 123.0(9) . . ? C17 C18 C19 118.8(8) . . ? C17 C18 C21 118.2(8) . . ? C19 C18 C21 123.0(8) . . ? O2 C19 C14 120.6(8) . . ? O2 C19 C18 121.0(8) . . ? C14 C19 C18 118.4(7) . . ? N4 C21 C18 128.4(8) . . ? N4 C22 C23 113.0(8) . . ? C22 C23 C24 118.6(8) . . ? C25 C24 C23 116.9(8) . . ? N3 C25 C24 110.1(7) . . ? N3 C26 C6 125.1(8) . . ? O4 C27 O3 123.2(9) . . ? O4 C27 C28 116.8(9) . . ? O3 C27 C28 119.9(9) . . ? O5 C29 O6 125.4(9) . . ? O5 C29 C30 118.1(9) . . ? O6 C29 C30 116.2(8) . . ? Cl1 C1S Cl3 111.7(6) . . ? Cl1 C1S Cl2 110.5(6) . . ? Cl3 C1S Cl2 108.2(6) . . ? _diffrn_measured_fraction_theta_max 0.797 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.797 _refine_diff_density_max 0.90 _refine_diff_density_min -0.86 _refine_diff_density_rms 0.15 #===END