Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Dean Giolando' 'Kristin Kirschbaum' 'Thomas C. Rosen' _publ_contact_author_name 'Prof Dean Giolando' _publ_contact_author_address ; Chemistry University of Toledo 2801 West Bancroft Toledo 43606 UNITED STATES OF AMERICA ; _publ_contact_author_email 'DGIOLAN@UOFT02.UTOLEDO.EDU' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Homoleptic Phenolate Complexes of Zirconium(IV): Syntheses and Structural Characterization of the First Six Coordinate Complexes ; _publ_section_acknowledgements ; We thank the College of Arts and Sciences of the University of Toledo for generous financial support of the X-ray diffraction facility. ; data_[Na(THF)2]2[Zr(OC6H4-2-Cl)6] _database_code_CSD 185537 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H56 Cl6 Na2 O10 Zr' _chemical_formula_weight 1190.87 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' 'Na' 'Na' 0.0362 0.0249 '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' 'Zr' 'Zr' -2.9673 0.5597 '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 10.8102(2) _cell_length_b 12.1126(3) _cell_length_c 12.2598(2) _cell_angle_alpha 111.212(1) _cell_angle_beta 109.659(1) _cell_angle_gamma 96.699(1) _cell_volume 1356.35(5) _cell_formula_units_Z 1 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 7940 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 26.88 _exptl_crystal_description '?' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method '?' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 0.570 _exptl_absorpt_correction_type 'Empirical :Multipole Expansion (Blessing, 1995)' _exptl_absorpt_correction_T_min 0.854298 _exptl_absorpt_correction_T_max 0.991925 _exptl_absorpt_process_details ? _exptl_special_details ; The decay correction was applied simultaneously with the absorption correction in sadabs. No formal measure of the extent of decay is printed out by this program. The final unit cell is obtained from the refinement of the XYZ weighted centroids of reflections above 20 \s(I). ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Sealed Tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD detector Smart Platform' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16012 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 30.11 _reflns_number_total 7139 _reflns_number_gt 5771 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL and the Toledo cifomatic' _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. Two C-atoms of one of the THF rings bonded to Na are disordered over two positions with equal occupancy. ; _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^)+(0.0496P)^2^+0.2280P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7139 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0949 _refine_ls_wR_factor_gt 0.0900 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 Zr1 Zr 0.0000 0.0000 0.5000 0.02184(7) Uani 1.000000 2 d S . . Cl1 Cl 0.13279(6) 0.32161(5) 0.37822(6) 0.04386(13) Uani 1.000000 1 d . . . Cl2 Cl 0.06899(8) -0.38492(5) 0.41284(6) 0.05757(18) Uani 1.000000 1 d . . . Cl3 Cl 0.06727(6) -0.03533(5) 0.86622(5) 0.04333(13) Uani 1.000000 1 d . . . Na1 Na 0.12396(8) -0.16855(7) 0.64229(7) 0.03408(18) Uani 1.000000 1 d . . . O1 O 0.11669(13) 0.13510(12) 0.48074(13) 0.0318(3) Uani 1.000000 1 d . . . O2 O 0.11325(13) -0.12391(11) 0.45858(12) 0.0285(3) Uani 1.000000 1 d . . . O3 O 0.12050(13) 0.05805(11) 0.69044(12) 0.0287(3) Uani 1.000000 1 d . . . O4 O 0.35505(16) -0.08032(17) 0.70591(15) 0.0527(4) Uani 1.000000 1 d . . . O5 O 0.20627(18) -0.30208(15) 0.73892(15) 0.0471(4) Uani 1.000000 1 d . . . C1 C 0.24314(19) 0.20157(16) 0.51987(18) 0.0294(4) Uani 1.000000 1 d . . . C2 C 0.2688(2) 0.29473(17) 0.4814(2) 0.0331(4) Uani 1.000000 1 d . . . C3 C 0.4003(2) 0.3673(2) 0.5245(2) 0.0460(6) Uani 1.000000 1 d . . . C4 C 0.5093(2) 0.3484(2) 0.6055(3) 0.0530(6) Uani 1.000000 1 d . . . C5 C 0.4875(2) 0.2551(2) 0.6433(2) 0.0512(6) Uani 1.000000 1 d . . . C6 C 0.3571(2) 0.1832(2) 0.6012(2) 0.0401(5) Uani 1.000000 1 d . . . C7 C 0.12127(18) -0.19721(17) 0.35077(17) 0.0289(4) Uani 1.000000 1 d . . . C8 C 0.1039(2) -0.32313(19) 0.31512(19) 0.0362(4) Uani 1.000000 1 d . . . C9 C 0.1095(2) -0.4012(2) 0.2021(2) 0.0498(6) Uani 1.000000 1 d . . . C10 C 0.1315(2) -0.3538(3) 0.1216(2) 0.0576(7) Uani 1.000000 1 d . . . C11 C 0.1493(2) -0.2308(3) 0.1547(2) 0.0542(7) Uani 1.000000 1 d . . . C12 C 0.1454(2) -0.1516(2) 0.2681(2) 0.0391(5) Uani 1.000000 1 d . . . C13 C 0.17050(19) 0.14297(17) 0.81213(17) 0.0284(4) Uani 1.000000 1 d . . . C14 C 0.1547(2) 0.11416(17) 0.90835(18) 0.0324(4) Uani 1.000000 1 d . . . C15 C 0.2028(3) 0.2007(2) 1.0346(2) 0.0458(5) Uani 1.000000 1 d . . . C16 C 0.2707(3) 0.3197(2) 1.0688(2) 0.0541(6) Uani 1.000000 1 d . . . C17 C 0.2882(3) 0.3508(2) 0.9758(2) 0.0535(6) Uani 1.000000 1 d . . . C18 C 0.2386(2) 0.26420(18) 0.8492(2) 0.0393(5) Uani 1.000000 1 d . . . C19 C 0.4508(3) -0.0182(4) 0.8345(3) 0.0768(10) Uani 1.000000 1 d . . . C20 C 0.5830(3) -0.0109(4) 0.8372(3) 0.0983(14) Uani 1.000000 1 d . . . C21 C 0.5691(3) -0.1037(3) 0.7127(3) 0.0729(9) Uani 1.000000 1 d . . . C22 C 0.4251(2) -0.1215(2) 0.6243(2) 0.0488(6) Uani 1.000000 1 d . . . C23 C 0.2062(4) -0.2970(3) 0.8567(3) 0.0673(8) Uani 1.000000 1 d . . . C24A C 0.3411(5) -0.3337(5) 0.9153(4) 0.0428(10) Uiso 0.500000 1 d P . . C24B C 0.2715(6) -0.3897(5) 0.8827(5) 0.0589(13) Uiso 0.500000 1 d P . . C25A C 0.3521(8) -0.4156(7) 0.8043(7) 0.075(2) Uiso 0.500000 1 d P . . C25B C 0.3093(6) -0.4515(5) 0.7839(5) 0.0401(11) Uiso 0.500000 1 d P . . C26 C 0.2829(3) -0.3859(3) 0.6984(3) 0.0591(7) Uani 1.000000 1 d . . . H3A H 0.4140 0.4289 0.4980 0.055 Uiso 1.000000 1 calc R . . H4A H 0.5970 0.3974 0.6352 0.064 Uiso 1.000000 1 calc R . . H5A H 0.5615 0.2409 0.6973 0.061 Uiso 1.000000 1 calc R . . H6A H 0.3448 0.1213 0.6275 0.048 Uiso 1.000000 1 calc R . . H9A H 0.0985 -0.4846 0.1812 0.060 Uiso 1.000000 1 calc R . . H10A H 0.1343 -0.4051 0.0453 0.069 Uiso 1.000000 1 calc R . . H11A H 0.1644 -0.1991 0.1001 0.065 Uiso 1.000000 1 calc R . . H12A H 0.1589 -0.0680 0.2889 0.047 Uiso 1.000000 1 calc R . . H15A H 0.1894 0.1786 1.0958 0.055 Uiso 1.000000 1 calc R . . H16A H 0.3043 0.3784 1.1534 0.065 Uiso 1.000000 1 calc R . . H17A H 0.3338 0.4310 0.9984 0.064 Uiso 1.000000 1 calc R . . H18A H 0.2510 0.2873 0.7883 0.047 Uiso 1.000000 1 calc R . . H19A H 0.4356 -0.0623 0.8830 0.092 Uiso 1.000000 1 calc R . . H19B H 0.4408 0.0638 0.8730 0.092 Uiso 1.000000 1 calc R . . H20A H 0.6397 -0.0274 0.9066 0.118 Uiso 1.000000 1 calc R . . H20B H 0.6250 0.0707 0.8503 0.118 Uiso 1.000000 1 calc R . . H21A H 0.5822 -0.1799 0.7177 0.087 Uiso 1.000000 1 calc R . . H21B H 0.6342 -0.0738 0.6846 0.087 Uiso 1.000000 1 calc R . . H22A H 0.4236 -0.0733 0.5758 0.059 Uiso 1.000000 1 calc R . . H22B H 0.3826 -0.2075 0.5648 0.059 Uiso 1.000000 1 calc R . . H23A H 0.1259 -0.3549 0.8422 0.081 Uiso 1.000000 1 calc R . . H23B H 0.2096 -0.2149 0.9126 0.081 Uiso 1.000000 1 calc R . . H24A H 0.4197 -0.2621 0.9655 0.051 Uiso 0.500000 1 calc R . . H24B H 0.3321 -0.3740 0.9688 0.051 Uiso 0.500000 1 calc R . . H24C H 0.3515 -0.3500 0.9634 0.071 Uiso 0.500000 1 calc R . . H24D H 0.2086 -0.4479 0.8899 0.071 Uiso 0.500000 1 calc R . . H25A H 0.3103 -0.4999 0.7841 0.090 Uiso 0.500000 1 calc R . . H25B H 0.4474 -0.4072 0.8191 0.090 Uiso 0.500000 1 calc R . . H25C H 0.2555 -0.5368 0.7364 0.048 Uiso 0.500000 1 calc R . . H25D H 0.4050 -0.4491 0.8181 0.048 Uiso 0.500000 1 calc R . . H26A H 0.3491 -0.3481 0.6763 0.071 Uiso 1.000000 1 calc R . . H26B H 0.2222 -0.4602 0.6236 0.071 Uiso 1.000000 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 Zr1 0.02596(13) 0.01742(11) 0.02144(12) 0.00762(9) 0.00988(9) 0.00516(9) Cl1 0.0496(3) 0.0336(3) 0.0523(3) 0.0249(2) 0.0196(3) 0.0071(2) Cl2 0.0927(5) 0.0263(3) 0.0433(3) 0.0141(2) 0.0177(3) 0.0133(3) Cl3 0.0614(3) 0.0352(3) 0.0393(3) 0.0159(2) 0.0284(3) 0.0100(2) Na1 0.0436(4) 0.0327(4) 0.0324(4) 0.0172(3) 0.0175(4) 0.0159(3) O1 0.0314(7) 0.0271(7) 0.0354(7) 0.0137(6) 0.0134(6) 0.0026(5) O2 0.0354(7) 0.0254(6) 0.0260(6) 0.0092(5) 0.0150(6) 0.0120(5) O3 0.0323(7) 0.0261(6) 0.0225(6) 0.0072(5) 0.0097(5) 0.0058(5) O4 0.0392(9) 0.0787(13) 0.0369(8) 0.0206(8) 0.0151(7) 0.0204(8) O5 0.0685(11) 0.0483(9) 0.0396(8) 0.0266(7) 0.0263(8) 0.0302(8) C1 0.0318(9) 0.0224(8) 0.0317(9) 0.0067(7) 0.0167(8) 0.0043(7) C2 0.0352(10) 0.0246(9) 0.0398(11) 0.0103(8) 0.0203(9) 0.0050(8) C3 0.0464(13) 0.0294(10) 0.0615(15) 0.0126(10) 0.0317(12) 0.0016(9) C4 0.0329(12) 0.0406(13) 0.0676(17) 0.0054(12) 0.0230(12) -0.0005(10) C5 0.0327(11) 0.0515(14) 0.0542(14) 0.0115(12) 0.0127(11) 0.0108(10) C6 0.0380(11) 0.0387(11) 0.0427(12) 0.0164(9) 0.0161(10) 0.0117(9) C7 0.0241(9) 0.0327(10) 0.0248(9) 0.0073(7) 0.0085(7) 0.0112(7) C8 0.0339(10) 0.0332(10) 0.0300(10) 0.0066(8) 0.0069(8) 0.0113(8) C9 0.0401(12) 0.0382(12) 0.0416(12) -0.0066(10) 0.0087(10) 0.0110(10) C10 0.0426(13) 0.0670(17) 0.0354(12) -0.0076(12) 0.0187(10) 0.0070(12) C11 0.0457(13) 0.0751(18) 0.0352(12) 0.0133(12) 0.0236(11) 0.0056(12) C12 0.0377(11) 0.0440(12) 0.0342(11) 0.0132(9) 0.0182(9) 0.0081(9) C13 0.0308(9) 0.0263(9) 0.0233(8) 0.0077(7) 0.0079(7) 0.0102(7) C14 0.0394(11) 0.0277(9) 0.0272(9) 0.0088(8) 0.0127(8) 0.0116(8) C15 0.0649(15) 0.0440(12) 0.0268(10) 0.0105(9) 0.0191(10) 0.0230(11) C16 0.0750(18) 0.0371(12) 0.0285(11) 0.0010(9) 0.0100(11) 0.0165(12) C17 0.0681(16) 0.0250(10) 0.0429(13) 0.0035(9) 0.0091(12) 0.0059(10) C18 0.0483(12) 0.0286(10) 0.0347(11) 0.0116(8) 0.0124(9) 0.0088(9) C19 0.0532(16) 0.117(3) 0.0365(14) 0.0133(16) 0.0112(12) 0.0272(17) C20 0.0459(16) 0.124(3) 0.0611(19) -0.012(2) 0.0065(14) 0.0191(19) C21 0.0389(14) 0.090(2) 0.0654(18) 0.0093(16) 0.0214(13) 0.0131(14) C22 0.0473(13) 0.0593(15) 0.0447(13) 0.0218(11) 0.0239(11) 0.0184(11) C23 0.113(2) 0.0703(19) 0.0522(15) 0.0402(14) 0.0469(17) 0.0553(18) C26 0.086(2) 0.0626(17) 0.0517(15) 0.0334(13) 0.0382(15) 0.0422(15) _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 Zr1 Na1 3.2634(8) 2_556 ? Zr1 Na1 3.2633(8) . ? Zr1 O1 2.0793(13) . ? Zr1 O1 2.0792(13) 2_556 ? Zr1 O2 2.0748(12) 2_556 ? Zr1 O2 2.0748(12) . ? Zr1 O3 2.0480(12) . ? Zr1 O3 2.0481(12) 2_556 ? Cl1 Na1 3.0326(10) 2_556 ? Cl1 C2 1.739(2) . ? Cl2 Na1 2.8831(10) . ? Cl2 C8 1.739(2) . ? Cl3 Na1 2.9451(9) . ? Cl3 C14 1.742(2) . ? Na1 Cl1 3.0325(10) 2_556 ? Na1 O1 2.6935(15) 2_556 ? Na1 O2 2.4696(14) . ? Na1 O3 2.5980(15) . ? Na1 O4 2.3354(18) . ? Na1 O5 2.4134(17) . ? O1 Na1 2.6935(15) 2_556 ? O1 C1 1.330(2) . ? O2 C7 1.337(2) . ? O3 C13 1.339(2) . ? O4 C19 1.409(3) . ? O4 C22 1.435(3) . ? O5 C23 1.423(3) . ? O5 C26 1.440(3) . ? C1 C2 1.405(3) . ? C3 C2 1.393(3) . ? C3 C4 1.367(4) . ? C3 H3A 0.9300 . ? C4 C5 1.392(4) . ? C4 H4A 0.9300 . ? C5 C6 1.382(3) . ? C5 H5A 0.9300 . ? C6 C1 1.400(3) . ? C6 H6A 0.9300 . ? C7 C8 1.396(3) . ? C7 C12 1.396(3) . ? C8 C9 1.392(3) . ? C9 C10 1.378(4) . ? C9 H9A 0.9300 . ? C10 C11 1.366(4) . ? C10 H10A 0.9300 . ? C11 C12 1.393(3) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.401(3) . ? C13 C18 1.394(3) . ? C14 C15 1.386(3) . ? C15 C16 1.379(3) . ? C15 H15A 0.9300 . ? C16 C17 1.385(4) . ? C16 H16A 0.9300 . ? C17 C18 1.388(3) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C20 1.410(4) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.476(4) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.504(4) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24A 1.587(5) . ? C23 C24B 1.467(6) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24A C25A 1.417(9) . ? C24A H24A 0.9700 . ? C24A H24B 0.9700 . ? C24B C25B 1.394(7) . ? C24B H24C 0.9700 . ? C24B H24D 0.9700 . ? C25A C26 1.456(8) . ? C25A H25A 0.9700 . ? C25A H25B 0.9700 . ? C25B C26 1.505(6) . ? C25B H25C 0.9700 . ? C25B H25D 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Na1 Zr1 Na1 180.0 . 2_556 ? Na1 Zr1 O1 124.66(4) . . ? Na1 Zr1 O1 55.34(4) . 2_556 ? Na1 Zr1 O1 124.66(4) 2_556 2_556 ? Na1 Zr1 O2 49.16(4) 2_556 2_556 ? Na1 Zr1 O2 130.84(4) . 2_556 ? Na1 Zr1 O2 49.16(4) . . ? Na1 Zr1 O3 52.73(4) . . ? Na1 Zr1 O3 52.73(4) 2_556 2_556 ? Na1 Zr1 O3 127.27(4) . 2_556 ? O1 Zr1 Na1 55.34(4) . 2_556 ? O1 Zr1 O1 179.999(2) 2_556 . ? O1 Zr1 O2 94.24(5) 2_556 2_556 ? O1 Zr1 O2 94.24(5) . . ? O1 Zr1 O2 85.76(5) . 2_556 ? O1 Zr1 O3 94.30(5) 2_556 2_556 ? O1 Zr1 O3 85.70(5) . 2_556 ? O1 Zr1 O3 94.30(5) . . ? O2 Zr1 Na1 130.84(4) . 2_556 ? O2 Zr1 O1 85.76(5) . 2_556 ? O2 Zr1 O2 180.0 . 2_556 ? O2 Zr1 O3 91.88(5) . 2_556 ? O2 Zr1 O3 88.12(5) 2_556 2_556 ? O2 Zr1 O3 88.12(5) . . ? O3 Zr1 Na1 127.27(4) . 2_556 ? O3 Zr1 O1 85.70(5) . 2_556 ? O3 Zr1 O2 91.88(5) . 2_556 ? O3 Zr1 O3 180.0 . 2_556 ? C2 Cl1 Na1 106.06(7) . 2_556 ? Na1 Cl2 C8 102.61(7) . . ? Na1 Cl3 C14 99.48(7) . . ? Zr1 Na1 Cl1 101.56(2) . 2_556 ? Zr1 Na1 Cl2 96.77(2) . . ? Zr1 Na1 Cl3 92.43(2) . . ? Zr1 Na1 O1 39.42(3) . 2_556 ? Zr1 Na1 O2 39.47(3) . . ? Zr1 Na1 O3 38.86(3) . . ? Zr1 Na1 O4 97.83(5) . . ? Zr1 Na1 O5 177.09(5) . . ? Cl1 Na1 O1 62.17(3) 2_556 2_556 ? Cl2 Na1 Cl1 80.55(3) . 2_556 ? Cl2 Na1 Cl3 151.31(4) . . ? Cl2 Na1 O1 88.69(4) . 2_556 ? Cl2 Na1 O2 66.45(4) . . ? Cl2 Na1 O3 134.15(4) . . ? Cl2 Na1 O4 101.08(5) . . ? Cl2 Na1 O5 80.96(4) . . ? Cl3 Na1 Cl1 70.99(2) . 2_556 ? Cl3 Na1 O1 81.33(4) . 2_556 ? Cl3 Na1 O2 130.87(4) . . ? Cl3 Na1 O3 63.94(3) . . ? Cl3 Na1 O4 104.50(5) . . ? Cl3 Na1 O5 88.78(4) . . ? O2 Na1 Cl1 118.20(4) . 2_556 ? O2 Na1 O1 66.22(4) . 2_556 ? O2 Na1 O3 68.86(4) . . ? O2 Na1 O4 79.71(6) . . ? O2 Na1 O5 139.81(6) . . ? O3 Na1 Cl1 112.85(4) . 2_556 ? O3 Na1 O1 64.04(4) . 2_556 ? O3 Na1 O4 80.36(6) . . ? O3 Na1 O5 143.77(6) . . ? O4 Na1 Cl1 160.23(6) . 2_556 ? O4 Na1 O1 137.22(6) . 2_556 ? O4 Na1 O5 84.42(7) . . ? O5 Na1 Cl1 76.34(5) . 2_556 ? O5 Na1 O1 138.36(6) . 2_556 ? Zr1 O1 Na1 85.24(5) . 2_556 ? Zr1 O1 C1 144.04(13) . . ? C1 O1 Na1 129.76(12) . 2_556 ? Zr1 O2 Na1 91.37(5) . . ? Zr1 O2 C7 134.07(11) . . ? Na1 O2 C7 127.67(11) . . ? Zr1 O3 Na1 88.41(5) . . ? Zr1 O3 C13 150.34(12) . . ? Na1 O3 C13 119.73(11) . . ? Na1 O4 C19 124.25(16) . . ? Na1 O4 C22 122.45(14) . . ? C19 O4 C22 109.43(18) . . ? Na1 O5 C23 125.41(14) . . ? Na1 O5 C26 125.49(13) . . ? C23 O5 C26 108.41(18) . . ? O1 C1 C2 121.24(18) . . ? O1 C1 C6 122.27(18) . . ? C6 C1 C2 116.49(18) . . ? Cl1 C2 C1 119.29(15) . . ? Cl1 C2 C3 118.85(17) . . ? C3 C2 C1 121.9(2) . . ? C2 C3 H3A 119.9 . . ? C4 C3 C2 120.2(2) . . ? C4 C3 H3A 119.9 . . ? C3 C4 C5 119.3(2) . . ? C3 C4 H4A 120.3 . . ? C5 C4 H4A 120.3 . . ? C4 C5 C6 120.6(2) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C1 C6 H6A 119.3 . . ? C5 C6 C1 121.5(2) . . ? C5 C6 H6A 119.3 . . ? O2 C7 C8 121.34(18) . . ? O2 C7 C12 121.56(18) . . ? C8 C7 C12 117.10(18) . . ? Cl2 C8 C7 118.78(15) . . ? Cl2 C8 C9 119.06(18) . . ? C7 C8 C9 122.1(2) . . ? C8 C9 C10 119.4(2) . . ? C8 C9 H9A 120.3 . . ? C10 C9 H9A 120.3 . . ? C9 C10 C11 119.5(2) . . ? C9 C10 H10A 120.2 . . ? C11 C10 H10A 120.2 . . ? C10 C11 C12 121.5(2) . . ? C10 C11 H11A 119.2 . . ? C12 C11 H11A 119.2 . . ? C7 C12 C11 120.3(2) . . ? C7 C12 H12A 119.9 . . ? C11 C12 H12A 119.9 . . ? O3 C13 C14 121.20(17) . . ? O3 C13 C18 122.07(18) . . ? C14 C13 C18 116.72(17) . . ? Cl3 C14 C13 118.46(14) . . ? Cl3 C14 C15 119.01(17) . . ? C13 C14 C15 122.52(19) . . ? C14 C15 C16 119.6(2) . . ? C14 C15 H15A 120.2 . . ? C16 C15 H15A 120.2 . . ? C15 C16 C17 119.2(2) . . ? C15 C16 H16A 120.4 . . ? C17 C16 H16A 120.4 . . ? C16 C17 C18 121.1(2) . . ? C16 C17 H17A 119.5 . . ? C18 C17 H17A 119.5 . . ? C13 C18 C17 120.9(2) . . ? C13 C18 H18A 119.5 . . ? C17 C18 H18A 119.5 . . ? O4 C19 C20 108.5(2) . . ? O4 C19 H19A 110.0 . . ? O4 C19 H19B 110.0 . . ? C20 C19 H19A 110.0 . . ? C20 C19 H19B 110.0 . . ? H19A C19 H19B 108.4 . . ? C19 C20 C21 107.4(3) . . ? C19 C20 H20A 110.2 . . ? C19 C20 H20B 110.2 . . ? C21 C20 H20A 110.2 . . ? C21 C20 H20B 110.2 . . ? H20A C20 H20B 108.5 . . ? C20 C21 C22 103.3(2) . . ? C20 C21 H21A 111.1 . . ? C20 C21 H21B 111.1 . . ? C22 C21 H21A 111.1 . . ? C22 C21 H21B 111.1 . . ? H21A C21 H21B 109.1 . . ? O4 C22 C21 105.6(2) . . ? O4 C22 H22A 110.6 . . ? O4 C22 H22B 110.6 . . ? C21 C22 H22A 110.6 . . ? C21 C22 H22B 110.6 . . ? H22A C22 H22B 108.8 . . ? O5 C23 C24A 102.9(3) . . ? O5 C23 C24B 107.3(3) . . ? O5 C23 H23A 111.2 . . ? O5 C23 H23B 111.2 . . ? C24A C23 C24B 30.8(3) . . ? C24A C23 H23A 111.2 . . ? C24A C23 H23B 111.2 . . ? C24B C23 H23A 81.6 . . ? C24B C23 H23B 131.9 . . ? H23A C23 H23B 109.1 . . ? C23 C24A C25A 102.6(4) . . ? C23 C24A H24A 111.3 . . ? C23 C24A H24B 111.3 . . ? C25A C24A H24A 111.3 . . ? C25A C24A H24B 111.3 . . ? H24A C24A H24B 109.2 . . ? C23 C24B C25B 109.9(4) . . ? C23 C24B H24C 109.7 . . ? C23 C24B H24D 109.7 . . ? C25B C24B H24C 109.7 . . ? C25B C24B H24D 109.7 . . ? H24C C24B H24D 108.2 . . ? C24A C25A C26 108.4(5) . . ? C24A C25A H25A 110.0 . . ? C24A C25A H25B 110.0 . . ? C26 C25A H25A 110.0 . . ? C26 C25A H25B 110.0 . . ? H25A C25A H25B 108.4 . . ? C24B C25B C26 106.2(4) . . ? C24B C25B H25C 110.5 . . ? C24B C25B H25D 110.5 . . ? C26 C25B H25C 110.5 . . ? C26 C25B H25D 110.5 . . ? H25C C25B H25D 108.7 . . ? O5 C26 C25A 107.8(4) . . ? O5 C26 C25B 107.0(3) . . ? O5 C26 H26A 110.2 . . ? O5 C26 H26B 110.2 . . ? C25A C26 C25B 19.8(4) . . ? C25A C26 H26A 110.2 . . ? C25A C26 H26B 110.2 . . ? C25B C26 H26A 126.7 . . ? C25B C26 H26B 92.7 . . ? H26A C26 H26B 108.5 . . ? _diffrn_measured_fraction_theta_max 0.893 _diffrn_reflns_theta_full 30.11 _diffrn_measured_fraction_theta_full 0.893 _refine_diff_density_max 0.441 _refine_diff_density_min -0.530 _refine_diff_density_rms 0.059 #========END=========== data_[NH2(CH3)2]2[Zr(OC6H4-2-Cl)6].2THF _database_code_CSD 185538 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H56 Cl6 N2 O8 Zr' _chemical_formula_weight 1092.87 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' 'Zr' 'Zr' -2.9673 0.5597 '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 10.604(2) _cell_length_b 13.538(3) _cell_length_c 18.379(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.43(3) _cell_angle_gamma 90.00 _cell_volume 2616.3(9) _cell_formula_units_Z 2 _cell_measurement_temperature 193(1) _cell_measurement_reflns_used 6756 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 27.05 _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_method ? _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.568 _exptl_absorpt_correction_type 'Empirical :Multipole Expansion (Blessing, 1995)' _exptl_absorpt_correction_T_min 0.796622 _exptl_absorpt_correction_T_max 0.991136 _exptl_absorpt_process_details ? _exptl_special_details ; The decay correction was applied simultaneously with the absorption correction in sadabs. No formal measure of the extent of decay is printed out by this program. The final unit cell is obtained from the refinement of the XYZ weighted centroids of reflections above 20 \s(I). ; _diffrn_ambient_temperature 193(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Sealed Tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD detector Smart platform' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17047 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 33.04 _reflns_number_total 6438 _reflns_number_gt 4627 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL and the Toledo cifomatic' _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^)+(0.0673P)^2^+0.3497P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom and difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6438 _refine_ls_number_parameters 303 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0707 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1206 _refine_ls_wR_factor_gt 0.1088 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.002 _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 Zr1 Zr 0.5000 0.0000 0.0000 0.02931(10) Uani 1.000000 2 d S . . Cl1 Cl 0.73517(10) -0.29219(7) -0.06859(5) 0.0826(3) Uani 1.000000 1 d . . . Cl2 Cl 0.79212(7) 0.07609(6) 0.16334(4) 0.0574(2) Uani 1.000000 1 d . . . Cl3 Cl 0.33665(7) -0.17189(5) 0.22089(4) 0.05284(19) Uani 1.000000 1 d . . . O1 O 0.60463(16) -0.12555(12) 0.01120(9) 0.0403(4) Uani 1.000000 1 d . . . O2 O 0.63494(16) 0.08168(13) 0.04278(9) 0.0415(4) Uani 1.000000 1 d . . . O3 O 0.39635(15) -0.02286(12) 0.10432(8) 0.0349(4) Uani 1.000000 1 d . . . O4 O 0.9590(2) 0.01343(14) -0.25383(11) 0.0570(5) Uani 1.000000 1 d . . . N1 N 0.8662(2) 0.05427(18) -0.10988(14) 0.0430(5) Uani 1.000000 1 d . . . C1 C 0.6656(2) -0.18328(18) 0.05314(13) 0.0359(5) Uani 1.000000 1 d . . . C2 C 0.7316(3) -0.2664(2) 0.02450(16) 0.0484(7) Uani 1.000000 1 d . . . C3 C 0.7941(3) -0.3288(2) 0.0679(2) 0.0694(10) Uani 1.000000 1 d . . . C4 C 0.7913(3) -0.3089(3) 0.1418(2) 0.0709(11) Uani 1.000000 1 d . . . C5 C 0.7284(3) -0.2265(3) 0.17132(17) 0.0641(9) Uani 1.000000 1 d . . . C6 C 0.6663(2) -0.1639(2) 0.12790(14) 0.0468(7) Uani 1.000000 1 d . . . C7 C 0.6941(2) 0.16616(19) 0.05149(13) 0.0371(6) Uani 1.000000 1 d . . . C8 C 0.7765(2) 0.1755(2) 0.10559(13) 0.0428(6) Uani 1.000000 1 d . . . C9 C 0.8466(3) 0.2607(2) 0.11242(17) 0.0605(8) Uani 1.000000 1 d . . . C10 C 0.8344(4) 0.3396(3) 0.0668(2) 0.0734(10) Uani 1.000000 1 d . . . C11 C 0.7501(3) 0.3340(2) 0.01506(19) 0.0681(9) Uani 1.000000 1 d . . . C12 C 0.6809(3) 0.2482(2) 0.00757(15) 0.0515(7) Uani 1.000000 1 d . . . C13 C 0.4014(2) 0.01247(16) 0.17195(12) 0.0299(5) Uani 1.000000 1 d . . . C14 C 0.3787(2) -0.04931(18) 0.23356(13) 0.0348(5) Uani 1.000000 1 d . . . C15 C 0.3869(3) -0.0147(2) 0.30357(14) 0.0470(7) Uani 1.000000 1 d . . . C16 C 0.4152(3) 0.0831(2) 0.31428(15) 0.0531(8) Uani 1.000000 1 d . . . C17 C 0.4353(3) 0.1459(2) 0.25480(14) 0.0462(6) Uani 1.000000 1 d . . . C18 C 0.4282(2) 0.11143(18) 0.18476(13) 0.0369(6) Uani 1.000000 1 d . . . C19 C 0.8816(3) -0.0361(2) -0.06658(17) 0.0556(8) Uani 1.000000 1 d . . . C20 C 0.9453(3) 0.1376(2) -0.09062(16) 0.0525(7) Uani 1.000000 1 d . . . C21 C 0.9412(3) -0.0861(2) -0.27744(18) 0.0607(8) Uani 1.000000 1 d . . . C22 C 0.9504(4) -0.0827(3) -0.3594(2) 0.0837(13) Uani 1.000000 1 d . . . C23 C 1.0196(5) 0.0106(3) -0.3808(2) 0.0982(15) Uani 1.000000 1 d . . . C24 C 1.0040(5) 0.0737(3) -0.3139(2) 0.0943(14) Uani 1.000000 1 d . . . H1A H 0.791(3) 0.0689(19) -0.1009(14) 0.034(7) Uiso 1.000000 1 d . . . H1B H 0.884(3) 0.039(3) -0.1551(19) 0.064(10) Uiso 1.000000 1 d . . . H3A H 0.8372 -0.3824 0.0513 0.083 Uiso 1.000000 1 calc R . . H4A H 0.8339 -0.3528 0.1753 0.085 Uiso 1.000000 1 calc R . . H5A H 0.7326 -0.2187 0.2219 0.077 Uiso 1.000000 1 calc R . . H6A H 0.6251 -0.1096 0.1450 0.056 Uiso 1.000000 1 calc R . . H9A H 0.9093 0.2647 0.1527 0.073 Uiso 1.000000 1 calc R . . H10A H 0.8869 0.3947 0.0744 0.088 Uiso 1.000000 1 calc R . . H11A H 0.7334 0.3859 -0.0180 0.082 Uiso 1.000000 1 calc R . . H12A H 0.6171 0.2454 -0.0322 0.062 Uiso 1.000000 1 calc R . . H15A H 0.3738 -0.0558 0.3424 0.056 Uiso 1.000000 1 calc R . . H16A H 0.4215 0.1091 0.3614 0.064 Uiso 1.000000 1 calc R . . H17A H 0.4538 0.2122 0.2640 0.055 Uiso 1.000000 1 calc R . . H18A H 0.4410 0.1535 0.1464 0.044 Uiso 1.000000 1 calc R . . H19A H 0.8206 -0.0843 -0.0871 0.083 Uiso 1.000000 1 calc R . . H19B H 0.8684 -0.0222 -0.0169 0.083 Uiso 1.000000 1 calc R . . H19C H 0.9660 -0.0616 -0.0672 0.083 Uiso 1.000000 1 calc R . . H20A H 0.9223 0.1902 -0.1248 0.079 Uiso 1.000000 1 calc R . . H20B H 1.0326 0.1198 -0.0920 0.079 Uiso 1.000000 1 calc R . . H20C H 0.9344 0.1591 -0.0421 0.079 Uiso 1.000000 1 calc R . . H21A H 0.8586 -0.1103 -0.2683 0.073 Uiso 1.000000 1 calc R . . H21B H 1.0066 -0.1284 -0.2523 0.073 Uiso 1.000000 1 calc R . . H22A H 0.8655 -0.0843 -0.3863 0.100 Uiso 1.000000 1 calc R . . H22B H 0.9957 -0.1407 -0.3731 0.100 Uiso 1.000000 1 calc R . . H23A H 1.1083 -0.0021 -0.3853 0.118 Uiso 1.000000 1 calc R . . H23B H 0.9782 0.0399 -0.4258 0.118 Uiso 1.000000 1 calc R . . H24A H 1.0849 0.1041 -0.2958 0.113 Uiso 1.000000 1 calc R . . H24B H 0.9433 0.1260 -0.3280 0.113 Uiso 1.000000 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 Zr1 0.02885(16) 0.03297(17) 0.02309(15) -0.00098(12) -0.00812(11) 0.00467(13) Cl1 0.0990(7) 0.0649(5) 0.0753(6) -0.0302(4) -0.0215(5) 0.0326(5) Cl2 0.0483(4) 0.0720(5) 0.0450(4) 0.0034(3) -0.0203(3) 0.0013(4) Cl3 0.0631(5) 0.0377(4) 0.0543(4) 0.0074(3) -0.0052(3) -0.0071(3) O1 0.0402(9) 0.0381(9) 0.0374(9) 0.0012(7) -0.0142(7) 0.0097(8) O2 0.0385(9) 0.0445(10) 0.0357(9) -0.0063(8) -0.0171(7) 0.0010(8) O3 0.0353(9) 0.0400(9) 0.0258(8) -0.0027(6) -0.0104(6) -0.0010(7) O4 0.0694(14) 0.0493(12) 0.0474(11) -0.0104(9) -0.0107(10) -0.0023(10) N1 0.0343(13) 0.0497(14) 0.0417(13) -0.0001(10) -0.0075(10) 0.0013(11) C1 0.0266(11) 0.0363(13) 0.0415(13) 0.0084(10) -0.0077(10) 0.0004(10) C2 0.0433(15) 0.0400(15) 0.0568(17) 0.0027(12) -0.0128(12) 0.0050(12) C3 0.0513(19) 0.0463(18) 0.104(3) 0.0181(18) -0.0162(18) 0.0145(15) C4 0.0456(17) 0.075(2) 0.084(2) 0.041(2) -0.0239(16) -0.0006(16) C5 0.0455(17) 0.094(3) 0.0477(17) 0.0282(17) -0.0145(13) -0.0091(18) C6 0.0356(14) 0.0587(17) 0.0427(15) 0.0067(13) -0.0071(11) 0.0031(13) C7 0.0322(12) 0.0447(14) 0.0321(12) -0.0091(10) -0.0045(10) 0.0010(11) C8 0.0350(13) 0.0543(16) 0.0355(13) -0.0079(12) -0.0088(10) 0.0008(12) C9 0.0503(17) 0.067(2) 0.0573(18) -0.0121(16) -0.0178(14) -0.0138(15) C10 0.073(2) 0.058(2) 0.083(2) -0.0077(19) -0.0143(19) -0.0216(18) C11 0.077(2) 0.0528(19) 0.068(2) 0.0069(16) -0.0153(18) -0.0071(17) C12 0.0534(17) 0.0511(17) 0.0449(15) 0.0011(13) -0.0125(13) 0.0033(14) C13 0.0249(10) 0.0362(13) 0.0264(10) -0.0005(9) -0.0052(8) 0.0026(9) C14 0.0315(12) 0.0349(13) 0.0350(12) 0.0026(10) -0.0067(10) -0.0017(10) C15 0.0465(15) 0.064(2) 0.0269(12) 0.0091(12) -0.0084(10) -0.0113(13) C16 0.0517(16) 0.071(2) 0.0322(13) -0.0103(13) -0.0093(12) -0.0157(15) C17 0.0454(15) 0.0471(16) 0.0435(15) -0.0115(12) -0.0041(12) -0.0107(12) C18 0.0358(13) 0.0388(13) 0.0339(13) 0.0029(10) -0.0032(10) -0.0002(10) C19 0.0433(16) 0.0547(17) 0.065(2) 0.0101(15) -0.0095(14) 0.0022(14) C20 0.0472(16) 0.0543(17) 0.0519(17) -0.0040(13) -0.0089(13) -0.0066(14) C21 0.0564(18) 0.0485(17) 0.071(2) -0.0143(15) -0.0162(15) -0.0017(14) C22 0.069(2) 0.110(3) 0.065(2) -0.038(2) -0.0194(18) 0.012(2) C23 0.144(5) 0.085(3) 0.064(2) 0.005(2) 0.007(3) 0.031(3) C24 0.132(4) 0.077(3) 0.071(3) 0.002(2) 0.001(3) -0.033(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 Zr1 O1 2.0256(16) . ? Zr1 O1 2.0256(16) 3_655 ? Zr1 O2 1.8967(16) 3_655 ? Zr1 O2 1.8966(16) . ? Zr1 O3 2.3505(18) 3_655 ? Zr1 O3 2.3505(18) . ? Cl1 C2 1.751(3) . ? Cl2 C8 1.709(3) . ? Cl3 C14 1.726(3) . ? O1 C1 1.222(3) . ? O2 C7 1.304(3) . ? O3 C13 1.327(3) . ? O4 C21 1.420(3) . ? O4 C24 1.499(4) . ? N1 C19 1.458(4) . ? N1 C20 1.423(3) . ? C1 C2 1.459(4) . ? C3 C2 1.285(4) . ? C3 C4 1.389(5) . ? C4 C5 1.441(5) . ? C5 C6 1.286(4) . ? C6 C1 1.398(4) . ? C7 C8 1.242(3) . ? C7 C12 1.370(4) . ? C8 C9 1.368(4) . ? C9 C10 1.354(5) . ? C10 C11 1.220(5) . ? C11 C12 1.371(4) . ? C13 C14 1.453(3) . ? C13 C18 1.383(3) . ? C14 C15 1.362(3) . ? C15 C16 1.366(4) . ? C16 C17 1.423(4) . ? C17 C18 1.362(3) . ? C21 C22 1.523(5) . ? C22 C23 1.537(6) . ? C23 C24 1.524(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 O1 Zr1 O1 180.00(9) 3_655 . ? O1 Zr1 O2 94.20(7) 3_655 3_655 ? O1 Zr1 O2 85.80(7) . 3_655 ? O1 Zr1 O2 94.20(7) . . ? O1 Zr1 O3 83.43(7) 3_655 . ? O1 Zr1 O3 96.57(7) . . ? O1 Zr1 O3 83.43(7) . 3_655 ? O1 Zr1 O3 96.57(7) 3_655 3_655 ? O2 Zr1 O1 85.80(7) . 3_655 ? O2 Zr1 O2 180.0 . 3_655 ? O2 Zr1 O3 98.39(7) . . ? O2 Zr1 O3 81.61(7) 3_655 . ? O2 Zr1 O3 98.39(7) 3_655 3_655 ? O2 Zr1 O3 81.61(7) . 3_655 ? O3 Zr1 O3 180.0 . 3_655 ? Zr1 O1 C1 147.00(17) . . ? Zr1 O2 C7 152.52(15) . . ? Zr1 O3 C13 138.63(14) . . ? C21 O4 C24 109.5(3) . . ? C19 N1 C20 120.6(2) . . ? O1 C1 C2 120.3(2) . . ? O1 C1 C6 115.8(2) . . ? C6 C1 C2 123.9(2) . . ? Cl1 C2 C1 125.30(19) . . ? Cl1 C2 C3 113.6(3) . . ? C3 C2 C1 121.1(3) . . ? C4 C3 C2 113.9(3) . . ? C3 C4 C5 126.0(3) . . ? C4 C5 C6 120.1(3) . . ? C5 C6 C1 115.0(3) . . ? O2 C7 C8 117.7(2) . . ? O2 C7 C12 128.9(2) . . ? C8 C7 C12 113.4(3) . . ? Cl2 C8 C7 114.7(2) . . ? Cl2 C8 C9 126.8(2) . . ? C7 C8 C9 118.5(3) . . ? C8 C9 C10 126.9(3) . . ? C9 C10 C11 115.8(3) . . ? C10 C11 C12 117.3(3) . . ? C7 C12 C11 128.0(3) . . ? O3 C13 C14 122.1(2) . . ? O3 C13 C18 119.4(2) . . ? C14 C13 C18 118.4(2) . . ? Cl3 C14 C13 120.95(18) . . ? Cl3 C14 C15 116.2(2) . . ? C13 C14 C15 122.8(2) . . ? C14 C15 C16 117.1(2) . . ? C15 C16 C17 121.4(3) . . ? C16 C17 C18 121.7(3) . . ? C13 C18 C17 118.5(2) . . ? O4 C21 C22 104.5(3) . . ? C21 C22 C23 111.8(3) . . ? C22 C23 C24 98.6(3) . . ? O4 C24 C23 111.5(3) . . ? _diffrn_measured_fraction_theta_max 0.650 _diffrn_reflns_theta_full 33.04 _diffrn_measured_fraction_theta_full 0.650 _refine_diff_density_max 0.435 _refine_diff_density_min -0.899 _refine_diff_density_rms 0.073