Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _audit_creation_date 11-01-05 _audit_creation_method CRYSTALS _publ_contact_letter ; These are the CIF format data (6 compounds) for the paper "Versatile routes to zirconium imido dichloride compounds" S R Dubberley, S. E. Evans, C. L. Boyd and P. Mountford ; _publ_contact_author_name 'Dr P. Mountford' _publ_contact_author_address ; Chemistry Research Laboratory Mansfied Road Oxford OX1 3TA UK ; _publ_contact_author_phone '+44 1865 285140' _contact_author_fax '+44 1865 285141' _publ_contact_author_email Philip.Mountford@chem.ox.ac.uk _publ_section_title ; New and versatile routes to zirconium imido dichloride compounds ; loop_ _publ_author_name 'Philip Mountford' 'Catherine L. Boyd' 'Stuart R. Dubberley' 'Simon Evans' data_COMPOUND_1 _database_code_depnum_ccdc_archive 'CCDC 260433' # Local code SRD6 _chemical_name_systematic ; [Zr2(mu-N-2,6-C6H3iPr2)2Cl4(THF)4] ; _chemical_name_common (Zr2(mu-N-2,6-C6H3iPr2)2Cl4(THF)4) _publ_section_exptl_refinement ; Molecules of SRD6 lie across crystallographic inversion centres. Both of the unique THF molecules were disordered over two sites with equal chemical occupancies. The disorder was modelled satisfactorily and the non-H atoms of these ligands were positionally and isotropically refined subject to vibrational restraints, and similarity restraints on the O-C and C-C distances and associated internal ring angles. ; _cell_length_a 11.1206(4) _cell_length_b 15.9555(6) _cell_length_c 12.6383(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.200(2) _cell_angle_gamma 90.00 _cell_volume 2239.0(1) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'Zr ' -2.9650 0.5600 17.8765 1.2762 10.9480 11.9160 5.4173 0.1176 3.6572 87.6627 2.0693 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum ' C40 H66 Cl4 N2 O4 Zr2 ' _chemical_formula_moiety ' C40 H66 Cl4 N2 O4 Zr2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 963.22 _cell_measurement_reflns_used 4385 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _cell_measurement_temperature 150 _cell_formula_units_Z 2 _exptl_crystal_description ' block ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.18 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.43 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method none _exptl_crystal_F_000 989.22 _exptl_absorpt_coefficient_mu 0.74 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.862 _exptl_absorpt_correction_T_max 0.875 _diffrn_standards_interval_time 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method CCD _diffrn_ambient_temperature 150 _diffrn_reflns_number 8483 _reflns_number_total 5128 _diffrn_reflns_av_R_equivalents 0.02 _reflns_number_gt 3178 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _refine_diff_density_min -0.87 _refine_diff_density_max 1.03 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 3178 _refine_ls_number_parameters 307 _refine_ls_R_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.0487 _refine_ls_goodness_of_fit_ref 1.1324 _refine_ls_shift/su_max 0.035007 _refine_ls_structure_factor_coef F _refine_ls_hydrogen_treatment 'riding model' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_hydrogens geometric _refine_ls_matrix_type full _refine_ls_number_restraints 182 _refine_ls_abs_structure_flack none _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 4 parameters, Carruthers & Watkin , 1979, 0.468 -.547 -.452E-01-.346 ; _refine_ls_extinction_method None _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SIR92 (Altomare, et al., 1994)' _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin et al., 1996) ; _computing_molecular_graphics 'CAMERON (Watkin, Prout and Pearce, 1996)' _computing_publication_material ; CRYSTALS Issue 10 (Watkin et al., 1996) ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Zr1 0.88063(5) 0.03073(4) 1.04689(5) 0.0315 1.0000 Uani Cl1 0.73005(14) -0.06176(11) 0.95530(15) 0.0513 1.0000 Uani Cl2 0.94877(17) 0.14093(14) 1.17354(18) 0.0684 1.0000 Uani O1 0.7687(5) -0.0061(3) 1.1902(4) 0.0662 1.0000 Uani O2 0.7226(4) 0.1291(3) 1.0157(4) 0.0593 1.0000 Uani N1 0.9901(4) 0.0554(3) 0.9189(4) 0.0320 1.0000 Uani C1 0.9531(5) 0.1189(4) 0.8451(5) 0.0385 1.0000 Uani C2 0.9858(7) 0.2032(4) 0.8636(6) 0.0494 1.0000 Uani C3 0.941(1) 0.2643(6) 0.7920(8) 0.0834 1.0000 Uani C4 0.8661(12) 0.2446(7) 0.707(1) 0.1086 1.0000 Uani C5 0.8397(9) 0.1612(7) 0.6850(8) 0.0969 1.0000 Uani C6 0.8807(7) 0.0976(5) 0.7521(6) 0.0610 1.0000 Uani C7 1.0723(11) 0.2302(5) 0.9522(7) 0.0890 1.0000 Uani C8 1.1898(12) 0.2588(7) 0.9106(9) 0.1062 1.0000 Uani C9 1.0234(12) 0.3019(6) 1.0164(9) 0.1106 1.0000 Uani C10 0.8498(9) 0.0079(7) 0.7210(7) 0.1167 1.0000 Uani C11 0.9205(11) -0.0160(8) 0.6264(7) 0.1256 1.0000 Uani C12 0.718(1) -0.0050(8) 0.6917(8) 0.1249 1.0000 Uani C13 0.7647(15) -0.0923(5) 1.2324(11) 0.0705 0.5000 Uani C14 0.6979(14) -0.0878(11) 1.3298(9) 0.0752 0.5000 Uani C15 0.5934(11) -0.0395(11) 1.2874(11) 0.0744 0.5000 Uani C16 0.6357(7) -0.0205(11) 1.1812(9) 0.0693 0.5000 Uani C131 0.812(1) -0.0321(11) 1.2982(7) 0.0708 0.5000 Uani C141 0.7051(14) -0.0627(9) 1.3513(12) 0.0778 0.5000 Uani C151 0.6287(12) 0.009(1) 1.3219(13) 0.0823 0.5000 Uani C161 0.7185(15) 0.0556(6) 1.2634(12) 0.0804 0.5000 Uani C17 0.732(1) 0.2174(5) 0.9826(15) 0.0712 0.5000 Uani C18 0.6088(11) 0.2525(7) 0.9804(18) 0.0774 0.5000 Uani C19 0.5355(11) 0.1812(9) 0.9395(15) 0.0755 0.5000 Uani C20 0.5928(7) 0.1091(7) 0.9954(15) 0.0674 0.5000 Uani C171 0.6832(13) 0.1929(7) 1.0923(7) 0.0600 0.5000 Uani C181 0.6281(15) 0.2632(7) 1.0314(11) 0.0639 0.5000 Uani C191 0.5796(14) 0.2229(9) 0.9322(11) 0.0637 0.5000 Uani C201 0.6591(12) 0.1509(8) 0.9142(7) 0.0597 0.5000 Uani H31 0.964 0.3241 0.8051 0.0989 1.0000 Uiso H41 0.8301 0.2897 0.660 0.1260 1.0000 Uiso H51 0.7923 0.1462 0.6181 0.1079 1.0000 Uiso H71 1.0894 0.1821 1.0015 0.1012 1.0000 Uiso H81 1.2475 0.2763 0.9700 0.1217 1.0000 Uiso H82 1.2241 0.2103 0.8723 0.1217 1.0000 Uiso H83 1.1759 0.3067 0.8603 0.1217 1.0000 Uiso H91 1.0819 0.3194 1.0752 0.1274 1.0000 Uiso H92 1.0046 0.3509 0.9690 0.1274 1.0000 Uiso H93 0.9476 0.2815 1.0467 0.1274 1.0000 Uiso H101 0.8707 -0.0294 0.7829 0.1335 1.0000 Uiso H111 0.9020 -0.0752 0.6050 0.1446 1.0000 Uiso H112 1.0083 -0.0108 0.6471 0.1446 1.0000 Uiso H113 0.8994 0.0223 0.5656 0.1446 1.0000 Uiso H121 0.702 -0.0648 0.6719 0.1436 1.0000 Uiso H122 0.671 0.0099 0.7542 0.1436 1.0000 Uiso H123 0.693 0.0320 0.6306 0.1436 1.0000 Uiso H131 0.8479 -0.1143 1.2484 0.0937 0.5000 Uiso H132 0.7213 -0.1296 1.1794 0.0937 0.5000 Uiso H141 0.7449 -0.0579 1.3881 0.0911 0.5000 Uiso H142 0.6735 -0.1443 1.3553 0.0911 0.5000 Uiso H151 0.5820 0.0128 1.3292 0.0901 0.5000 Uiso H152 0.5171 -0.0728 1.2842 0.0901 0.5000 Uiso H161 0.5944 0.0307 1.1515 0.0912 0.5000 Uiso H162 0.6172 -0.0692 1.1333 0.0912 0.5000 Uiso H1311 0.848 0.0171 1.3371 0.0937 0.5000 Uiso H1312 0.873 -0.0775 1.2943 0.0937 0.5000 Uiso H1411 0.7204 -0.0673 1.4298 0.0943 0.5000 Uiso H1412 0.6744 -0.1175 1.3225 0.0943 0.5000 Uiso H1511 0.6005 0.041 1.3842 0.1003 0.5000 Uiso H1512 0.5575 -0.008 1.2752 0.1003 0.5000 Uiso H1611 0.7832 0.0782 1.3137 0.1076 0.5000 Uiso H1612 0.6792 0.1029 1.2227 0.1076 0.5000 Uiso H171 0.786 0.2488 1.0347 0.0862 0.5000 Uiso H172 0.765 0.2209 0.9107 0.0862 0.5000 Uiso H181 0.5860 0.2693 1.0529 0.0935 0.5000 Uiso H182 0.6011 0.3019 0.9318 0.0935 0.5000 Uiso H191 0.4496 0.1876 0.9576 0.0903 0.5000 Uiso H192 0.5396 0.1756 0.8610 0.0903 0.5000 Uiso H201 0.5541 0.0992 1.0639 0.0810 0.5000 Uiso H202 0.5838 0.0578 0.9502 0.0810 0.5000 Uiso H1711 0.7550 0.2143 1.1351 0.0717 0.5000 Uiso H1712 0.6251 0.1673 1.1405 0.0717 0.5000 Uiso H1811 0.6874 0.3085 1.0179 0.0762 0.5000 Uiso H1812 0.5601 0.2870 1.0704 0.0762 0.5000 Uiso H1911 0.4943 0.2044 0.9377 0.0766 0.5000 Uiso H1912 0.5843 0.2637 0.8725 0.0766 0.5000 Uiso H2011 0.7183 0.1649 0.8602 0.0724 0.5000 Uiso H2012 0.6089 0.1021 0.8889 0.0724 0.5000 Uiso 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 0.0284(3) 0.0286(3) 0.0372(3) -0.0005(3) -0.00044(19) 0.0000(2) Cl1 0.0356(8) 0.051(1) 0.0675(11) -0.0169(8) 0.0010(7) -0.0094(7) Cl2 0.051(1) 0.0707(14) 0.0849(14) -0.0448(11) 0.0127(9) -0.0131(9) O1 0.075(3) 0.063(3) 0.064(3) 0.004(2) 0.032(2) -0.001(2) O2 0.041(2) 0.048(3) 0.088(3) 0.003(2) -0.001(2) 0.0113(19) N1 0.034(2) 0.029(2) 0.033(3) 0.0010(19) -0.0031(19) -0.0026(19) C1 0.039(3) 0.035(3) 0.041(3) 0.008(3) -0.011(3) 0.001(3) C2 0.060(4) 0.035(4) 0.052(4) 0.007(3) -0.004(3) -0.001(3) C3 0.109(8) 0.046(5) 0.091(7) 0.022(5) -0.029(6) 0.001(5) C4 0.13(1) 0.077(7) 0.109(9) 0.055(6) -0.054(7) 0.003(6) C5 0.113(8) 0.082(7) 0.088(7) 0.048(6) -0.060(6) -0.025(6) C6 0.070(5) 0.061(5) 0.050(4) 0.019(4) -0.018(4) -0.016(4) C7 0.158(8) 0.043(4) 0.061(5) 0.009(3) -0.030(5) -0.037(4) C8 0.171(8) 0.070(4) 0.074(4) 0.014(4) -0.029(5) -0.038(4) C9 0.186(8) 0.062(5) 0.079(5) 0.005(4) -0.027(5) -0.016(5) C10 0.179(8) 0.111(6) 0.054(4) 0.024(4) -0.048(5) -0.077(6) C11 0.195(8) 0.119(7) 0.059(4) 0.016(5) -0.029(5) -0.066(6) C12 0.175(8) 0.119(6) 0.073(5) 0.036(5) -0.057(5) -0.080(6) C13 0.079(5) 0.065(5) 0.070(5) 0.003(4) 0.032(4) -0.005(4) C14 0.084(5) 0.069(5) 0.075(5) 0.003(5) 0.032(5) -0.007(5) C15 0.081(5) 0.071(5) 0.074(5) 0.005(5) 0.032(5) -0.006(5) C16 0.075(5) 0.066(5) 0.069(4) 0.007(4) 0.031(4) -0.002(4) C131 0.080(4) 0.069(4) 0.067(4) 0.002(4) 0.030(4) -0.004(4) C141 0.088(5) 0.075(5) 0.073(5) -0.005(5) 0.032(5) -0.006(5) C151 0.092(6) 0.080(6) 0.079(6) -0.010(5) 0.035(5) -0.004(5) C161 0.088(7) 0.078(7) 0.079(7) -0.013(6) 0.038(6) -0.003(6) C17 0.050(4) 0.056(4) 0.106(5) 0.005(4) -0.009(4) 0.009(4) C18 0.053(5) 0.063(5) 0.114(6) 0.003(5) -0.015(5) 0.007(4) C19 0.050(5) 0.061(5) 0.114(6) 0.003(5) -0.011(5) 0.009(4) C20 0.045(4) 0.053(4) 0.103(5) 0.000(4) -0.006(4) 0.009(4) C171 0.046(4) 0.050(4) 0.083(5) -0.007(4) -0.004(4) 0.011(4) C181 0.053(5) 0.053(5) 0.084(5) -0.010(4) -0.009(4) 0.012(4) C191 0.053(5) 0.051(5) 0.086(5) -0.009(4) -0.012(4) 0.012(4) C201 0.045(4) 0.048(4) 0.084(5) -0.004(4) -0.008(4) 0.014(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zr1 . Zr1 2_757 3.1250(11) yes Zr1 . Cl1 . 2.4709(17) yes Zr1 . Cl2 . 2.4683(18) yes Zr1 . O1 . 2.329(4) yes Zr1 . O2 . 2.372(4) yes Zr1 . N1 . 2.115(5) yes Zr1 . N1 2_757 2.018(5) yes O1 . C13 . 1.477(5) yes O1 . C16 . 1.494(5) yes O1 . C131 . 1.480(5) yes O1 . C161 . 1.481(5) yes O2 . C17 . 1.475(5) yes O2 . C20 . 1.487(5) yes O2 . C171 . 1.487(5) yes O2 . C201 . 1.471(5) yes N1 . C1 . 1.422(7) yes C1 . C2 . 1.410(9) yes C1 . C6 . 1.427(9) yes C2 . C3 . 1.40(1) yes C2 . C7 . 1.499(11) yes C3 . C4 . 1.357(14) yes C4 . C5 . 1.388(15) yes C5 . C6 . 1.383(11) yes C6 . C10 . 1.519(13) yes C7 . C8 . 1.507(16) yes C7 . C9 . 1.521(15) yes C10 . C11 . 1.516(9) yes C10 . C12 . 1.504(8) yes C13 . C14 . 1.475(5) yes C14 . C15 . 1.470(5) yes C15 . C16 . 1.478(5) yes C131 . C141 . 1.476(5) yes C141 . C151 . 1.466(5) yes C151 . C161 . 1.473(5) yes C17 . C18 . 1.476(5) yes C18 . C19 . 1.477(5) yes C19 . C20 . 1.476(5) yes C171 . C181 . 1.475(5) yes C181 . C191 . 1.482(5) yes C191 . C201 . 1.476(5) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Zr1 2_757 Zr1 . Cl1 . 101.70(5) yes Zr1 2_757 Zr1 . Cl2 . 103.47(5) yes Cl1 . Zr1 . Cl2 . 154.79(6) yes Zr1 2_757 Zr1 . O1 . 135.90(14) yes Cl1 . Zr1 . O1 . 80.56(15) yes Cl2 . Zr1 . O1 . 80.41(15) yes Zr1 2_757 Zr1 . O2 . 141.40(14) yes Cl1 . Zr1 . O2 . 80.85(13) yes Cl2 . Zr1 . O2 . 80.45(14) yes O1 . Zr1 . O2 . 82.69(19) yes Zr1 2_757 Zr1 . N1 . 39.73(13) yes Cl1 . Zr1 . N1 . 99.02(13) yes Cl2 . Zr1 . N1 . 101.21(13) yes O1 . Zr1 . N1 . 175.52(19) yes O2 . Zr1 . N1 . 101.67(19) yes Zr1 2_757 Zr1 . N1 2_757 42.06(13) yes Cl1 . Zr1 . N1 2_757 98.61(14) yes Cl2 . Zr1 . N1 2_757 99.03(14) yes O1 . Zr1 . N1 2_757 93.85(19) yes O2 . Zr1 . N1 2_757 176.54(19) yes N1 . Zr1 . N1 2_757 81.8(2) yes Zr1 . O1 . C13 . 122.9(5) yes Zr1 . O1 . C16 . 123.3(5) yes C13 . O1 . C16 . 80.5(9) yes Zr1 . O1 . C131 . 129.0(5) yes Zr1 . O1 . C161 . 123.7(5) yes C131 . O1 . C161 . 73.9(9) yes Zr1 . O2 . C17 . 128.1(5) yes Zr1 . O2 . C20 . 126.1(5) yes C17 . O2 . C20 . 103.8(6) yes Zr1 . O2 . C171 . 125.9(5) yes Zr1 . O2 . C201 . 128.0(5) yes C171 . O2 . C201 . 105.2(6) yes Zr1 . N1 . Zr1 2_757 98.2(2) yes Zr1 . N1 . C1 . 118.4(4) yes Zr1 2_757 N1 . C1 . 143.3(4) yes N1 . C1 . C2 . 120.6(5) yes N1 . C1 . C6 . 120.0(6) yes C2 . C1 . C6 . 119.5(6) yes C1 . C2 . C3 . 118.4(7) yes C1 . C2 . C7 . 123.1(6) yes C3 . C2 . C7 . 118.3(7) yes C2 . C3 . C4 . 122.1(9) yes C3 . C4 . C5 . 119.5(8) yes C4 . C5 . C6 . 121.5(9) yes C1 . C6 . C5 . 118.8(8) yes C1 . C6 . C10 . 123.1(7) yes C5 . C6 . C10 . 118.0(8) yes C2 . C7 . C8 . 111.1(8) yes C2 . C7 . C9 . 112.4(9) yes C8 . C7 . C9 . 107.5(8) yes C6 . C10 . C11 . 108.8(8) yes C6 . C10 . C12 . 113.3(9) yes C11 . C10 . C12 . 108.2(9) yes O1 . C13 . C14 . 106.4(7) yes C14 . C13 . C131 . 69.3(10) yes C13 . C14 . C15 . 98.4(7) yes C14 . C15 . C16 . 98.8(7) yes O1 . C16 . C15 . 109.1(7) yes O1 . C131 . C141 . 106.7(7) yes C131 . C141 . C151 . 95.3(7) yes C141 . C151 . C161 . 96.9(7) yes O1 . C161 . C151 . 105.7(7) yes O2 . C17 . C18 . 106.8(7) yes C17 . C18 . C19 . 102.0(7) yes C18 . C19 . C20 . 102.6(7) yes O2 . C20 . C19 . 107.7(6) yes O2 . C171 . C181 . 108.1(6) yes C171 . C181 . C191 . 103.5(7) yes C181 . C191 . C201 . 106.0(6) yes O2 . C201 . C191 . 108.2(6) yes #===end data_COMPOUND_2 _database_code_depnum_ccdc_archive 'CCDC 260434' # Local code SRD9 _chemical_name_systematic ; [Zr2(mu-N-2,6-C6H3Me2)2Cl4(THF)4] ; _chemical_name_common (Zr2(mu-N-2,6-C6H3Me2)2Cl4(THF)4) _publ_section_exptl_refinement ; Molecules of SRD6 lie across crystallographic 2/m symmetry sites with the Zr2N2O4 coordination cores lying on the mirror planes and perpendicular two-fold axes bisecting the Zr...Zr vectors. One quarter of each molecule of SRD9 is crystallographically unique. The THF molecules were disordered over two sites with equal chemical occupancies, and this disorder was modelled satisfactorily. ; _cell_length_a 12.7820(3) _cell_length_b 17.5806(5) _cell_length_c 15.9014(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3573.3(2) _symmetry_cell_setting 'Orthorhombic ' _symmetry_space_group_name_H-M 'C m c a ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,z x,-y,-z -x+1/2,y+1/2,z x+1/2,-y+1/2,-z x,-y+1/2,z+1/2 -x,y+1/2,-z+1/2 x+1/2,-y,z+1/2 -x+1/2,y,-z+1/2 -x,-y+1/2,z+1/2 x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 x+1/2,y,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'Zr ' -2.9650 0.5600 17.8765 1.2762 10.9480 11.9160 5.4173 0.1176 3.6572 87.6627 2.0693 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum ' C32 H50 Cl4 N2 O4 Zr2 ' _chemical_formula_moiety ' C32 H50 Cl4 N2 O4 Zr2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 851.00 _cell_measurement_reflns_used 2140 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_min 0.18 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_max 0.26 _exptl_crystal_density_diffrn 1.58 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method none _exptl_crystal_F_000 1722.41 _exptl_absorpt_coefficient_mu 0.92 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.817 _exptl_absorpt_correction_T_max 0.847 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_standards_interval_time 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method CCD _diffrn_ambient_temperature 150 _diffrn_reflns_number 4063 _reflns_number_total 2138 _diffrn_reflns_av_R_equivalents 0.019 _reflns_number_gt 1829 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min 0 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _refine_diff_density_min -0.46 _refine_diff_density_max 0.54 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 1829 _refine_ls_number_parameters 129 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0258 _refine_ls_goodness_of_fit_ref 1.0221 _refine_ls_shift/su_max 0.009 _refine_ls_structure_factor_coef F _refine_ls_extinction_coef 49.4(80) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' _refine_ls_hydrogen_treatment 'riding model' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_hydrogens geometric _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_abs_structure_flack none _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 0.459 0.353E-010.202 ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Zr1 0.0000 0.064707(13) 0.431031(15) 0.0154 1.0000 Uani Cl1 -0.18644(3) 0.09114(3) 0.40450(3) 0.0248 1.0000 Uani N1 0.0000 0.05215(12) 0.56123(13) 0.0165 1.0000 Uani O1 0.0000 0.1996(1) 0.44766(12) 0.0223 1.0000 Uani O2 0.0000 0.05457(11) 0.28149(12) 0.0232 1.0000 Uani C1 0.0000 0.11201(14) 0.62145(15) 0.0171 1.0000 Uani C2 0.09535(14) 0.1423(1) 0.65176(11) 0.0207 1.0000 Uani C3 0.09300(16) 0.20419(11) 0.70705(12) 0.0261 1.0000 Uani C4 -0.000000(7) 0.23598(17) 0.73442(19) 0.0300 1.0000 Uani C5 0.19998(15) 0.11092(12) 0.62622(13) 0.0273 1.0000 Uani C6 0.09307(16) 0.24769(11) 0.46006(16) 0.0327 1.0000 Uani C7 0.0534(4) 0.3287(3) 0.4628(4) 0.0350 0.5000 Uani C71 0.0491(4) 0.3173(3) 0.5087(4) 0.0325 0.5000 Uani C8 -0.09222(16) 0.04417(18) 0.22793(14) 0.0428 1.0000 Uani C9 -0.0541(7) 0.0226(5) 0.1418(6) 0.0392 0.5000 Uani C91 -0.0564(8) -0.0058(5) 0.1585(5) 0.0360 0.5000 Uani H31 0.16063 0.22616 0.72727 0.0321 1.0000 Uiso H41 -0.000000 0.28078 0.77317 0.0343 1.0000 Uiso H51 0.25662 0.14048 0.65475 0.0324 1.0000 Uiso H52 0.20481 0.05623 0.64306 0.0324 1.0000 Uiso H53 0.20821 0.11532 0.56387 0.0324 1.0000 Uiso H61 0.12849 0.23374 0.51397 0.0431 1.0000 Uiso H62 0.14317 0.24123 0.41229 0.0431 1.0000 Uiso H71 0.1014 0.3621 0.4961 0.0470 0.5000 Uiso H72 0.0434 0.3507 0.4054 0.0470 0.5000 Uiso H711 0.0386 0.3053 0.5696 0.0433 0.5000 Uiso H712 0.0959 0.3626 0.5032 0.0433 0.5000 Uiso H81 -0.13773 0.00359 0.25250 0.0578 1.0000 Uiso H82 -0.13235 0.09292 0.22468 0.0578 1.0000 Uiso H91 -0.0960 -0.0209 0.1194 0.0622 0.5000 Uiso H92 -0.0568 0.0660 0.1012 0.0622 0.5000 Uiso H911 -0.0583 -0.0605 0.1755 0.0478 0.5000 Uiso H912 -0.1018 0.0020 0.1081 0.0478 0.5000 Uiso 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 0.01127(12) 0.01754(13) 0.01742(13) -0.00024(9) 0.0000 0.0000 Cl1 0.01360(19) 0.0309(2) 0.0299(2) -0.00516(18) -0.00254(16) 0.00282(16) N1 0.0114(9) 0.020(1) 0.0179(9) -0.0024(8) 0.0000 0.0000 O1 0.0183(8) 0.0185(8) 0.030(1) 0.0031(7) 0.0000 0.0000 O2 0.0148(8) 0.0343(11) 0.0206(9) 0.0013(8) 0.0000 0.0000 C1 0.0170(11) 0.0185(11) 0.0157(11) 0.0006(9) 0.0000 0.0000 C2 0.0213(9) 0.0212(8) 0.0197(8) -0.0015(7) -0.0031(7) -0.0004(7) C3 0.027(1) 0.0256(9) 0.0255(9) -0.0054(7) -0.0050(8) -0.0031(8) C4 0.0360(15) 0.0269(14) 0.0271(14) -0.0091(11) 0.0000 0.0000 C5 0.0190(9) 0.030(1) 0.033(1) -0.0076(8) -0.0046(8) -0.0009(8) C6 0.0246(9) 0.0242(9) 0.0493(12) -0.0030(9) -0.0031(9) -0.0052(8) C7 0.036(2) 0.023(2) 0.046(3) -0.002(2) 0.008(3) -0.0046(18) C71 0.037(2) 0.023(2) 0.038(3) -0.006(2) -0.007(2) 0.0019(18) C8 0.019(1) 0.0805(18) 0.0292(11) -0.0138(11) -0.0058(8) 0.002(1) C9 0.025(3) 0.064(6) 0.029(4) -0.003(3) -0.002(3) 0.002(4) C91 0.033(3) 0.049(4) 0.026(4) -0.011(3) 0.000(3) -0.013(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zr1 . Cl1 . 2.4643(4) yes Zr1 . Cl1 5_555 2.4643(4) yes Zr1 . N1 . 2.082(2) yes Zr1 . N1 2_556 2.058(2) yes Zr1 . O1 . 2.3869(18) yes Zr1 . O2 . 2.3845(19) yes N1 . C1 . 1.423(3) yes O1 . C6 . 1.472(2) yes O1 . C6 5_555 1.472(2) yes O2 . C8 . 1.466(2) yes O2 . C8 5_555 1.466(2) yes C1 . C2 . 1.415(2) yes C1 . C2 5_555 1.415(2) yes C2 . C3 . 1.399(3) yes C2 . C5 . 1.503(3) yes C3 . C4 . 1.384(2) yes C6 . C7 . 1.512(5) yes C6 . C71 . 1.553(5) yes C7 . C71 5_555 1.513(6) yes C8 . C9 . 1.50(1) yes C8 . C91 . 1.48(1) yes C9 . C91 5_555 1.521(6) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Zr1 2_556 Zr1 . Cl1 . 104.748(12) yes Zr1 2_556 Zr1 . Cl1 5_555 104.748(12) yes Cl1 . Zr1 . Cl1 5_555 150.49(2) yes Zr1 2_556 Zr1 . N1 . 39.96(6) yes Cl1 . Zr1 . N1 . 100.965(16) yes Cl1 5_555 Zr1 . N1 . 100.965(16) yes Zr1 2_556 Zr1 . N1 2_556 40.53(6) yes Cl1 . Zr1 . N1 2_556 101.447(16) yes Cl1 5_555 Zr1 . N1 2_556 101.447(16) yes N1 . Zr1 . N1 2_556 80.49(9) yes Zr1 2_556 Zr1 . O1 . 129.69(5) yes Cl1 . Zr1 . O1 . 80.303(15) yes Cl1 5_555 Zr1 . O1 . 80.303(15) yes N1 . Zr1 . O1 . 89.72(7) yes N1 2_556 Zr1 . O1 . 170.21(7) yes Zr1 2_556 Zr1 . O2 . 129.67(5) yes Cl1 . Zr1 . O2 . 80.989(15) yes Cl1 5_555 Zr1 . O2 . 80.989(15) yes N1 . Zr1 . O2 . 169.63(7) yes N1 2_556 Zr1 . O2 . 89.14(8) yes O1 . Zr1 . O2 . 100.65(7) yes Zr1 . N1 . Zr1 2_556 99.51(9) yes Zr1 . N1 . C1 . 126.21(16) yes Zr1 2_556 N1 . C1 . 134.27(17) yes Zr1 . O1 . C6 . 125.8(1) yes Zr1 . O1 . C6 5_555 125.8(1) yes C6 . O1 . C6 5_555 107.8(2) yes Zr1 . O2 . C8 . 126.1(1) yes Zr1 . O2 . C8 5_555 126.1(1) yes C8 . O2 . C8 5_555 107.1(2) yes N1 . C1 . C2 . 120.51(11) yes N1 . C1 . C2 5_555 120.51(11) yes C2 . C1 . C2 5_555 119.0(2) yes C1 . C2 . C3 . 119.22(18) yes C1 . C2 . C5 . 122.46(16) yes C3 . C2 . C5 . 118.32(16) yes C2 . C3 . C4 . 122.01(19) yes C3 . C4 . C3 5_555 118.4(3) yes O1 . C6 . C7 . 105.9(2) yes O1 . C6 . C71 . 103.1(2) yes C6 . C7 . C71 5_555 100.3(3) yes C6 . C71 . C7 5_555 100.3(4) yes O2 . C8 . C9 . 107.4(4) yes O2 . C8 . C91 . 104.9(4) yes C8 . C9 . C91 5_555 103.0(8) yes C8 . C91 . C9 5_555 102.9(8) yes #===end data_COMPOUND_4 _database_code_depnum_ccdc_archive 'CCDC 260435' # Local code SRD12 _chemical_name_systematic ; [Zr2(mu-NC6F5)2Cl6(THF)2][Li(thf)3]2 ; _chemical_name_common (Zr2(mu-NC6F5)2Cl6(THF)2)(Li(thf)3)2 _publ_section_exptl_refinement ; no special requirements ; _cell_length_a 10.3615(2) _cell_length_b 11.7620(2) _cell_length_c 11.9942(2) _cell_angle_alpha 93.973(1) _cell_angle_beta 97.234(1) _cell_angle_gamma 106.1726(8) _cell_volume 1384.35(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 _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'F ' 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'Li ' -0.0003 0.0001 1.1282 3.9546 0.7508 1.0524 0.6175 85.3905 0.4653 168.2610 0.0377 International_Tables_Vol_IV_Table_2.2B 'Zr ' -2.9673 0.5597 17.8765 1.2762 10.9480 11.9160 5.4173 0.1176 3.6572 87.6627 2.0693 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 1 _chemical_formula_sum ' C44 H64 Cl6 F10 Li2 N2 O8 Zr2 ' _chemical_formula_moiety ' C44 H64 Cl6 F10 Li2 N2 O8 Zr2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 1348.02 _cell_measurement_reflns_used 5959 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _cell_measurement_temperature 150 _exptl_crystal_description ' wedge ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.24 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_max 0.34 _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method none _exptl_crystal_F_000 684.000 _exptl_absorpt_coefficient_mu 0.749 _diffrn_measurement_device_type ; Enraf Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR97 (Altomare et al, 1999) ; _diffrn_measurement_method CCD _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.84 _diffrn_standards_interval_time 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_ambient_temperature 150 _diffrn_reflns_number 11874 _reflns_number_total 6361 _diffrn_reflns_av_R_equivalents 0.04 _diffrn_reflns_theta_min 2.960 _diffrn_reflns_theta_max 27.599 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.392 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min -15 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _refine_diff_density_min -0.78 _refine_diff_density_max 0.65 _refine_ls_number_reflns 5331 _refine_ls_number_parameters 335 _refine_ls_wR_factor_ref 0.0278 _refine_ls_goodness_of_fit_ref 1.1258 _refine_ls_R_factor_all 0.0435 _refine_ls_wR_factor_all 0.0319 _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 5331 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_gt 0.0278 _refine_ls_shift/su_max 0.000229 _refine_ls_structure_factor_coef F _refine_ls_hydrogen_treatment 'riding model' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_hydrogens geometric _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_abs_structure_flack none _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method = Prince modified Chebychev polynomial, (Watkin, 1994) W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 0.503 -0.346 0.709E-01 -0.284 ; _refine_ls_extinction_coef 54.0(32) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_attached_hydrogens Zr1 Zr 0.10398(2) 0.010434(17) -0.091487(17) 0.0215 1.0000 Uani . Cl1 Cl 0.30481(5) 0.18303(5) -0.12058(5) 0.0291 1.0000 Uani . Cl2 Cl 0.16442(6) -0.14499(5) -0.20782(5) 0.0364 1.0000 Uani . Cl3 Cl -0.02087(6) 0.06558(5) -0.25820(5) 0.0320 1.0000 Uani . N1 N -0.05555(17) -0.11589(15) -0.03877(14) 0.0214 1.0000 Uani . O1 O 0.26366(16) -0.02550(13) 0.03882(14) 0.0277 1.0000 Uani . O2 O 0.04321(17) 0.31474(15) -0.37972(14) 0.0336 1.0000 Uani . O3 O 0.27187(18) 0.20858(16) -0.40158(16) 0.0379 1.0000 Uani . O4 O 0.30099(19) 0.43603(15) -0.23223(16) 0.0401 1.0000 Uani . Li1 Li 0.1863(4) 0.2679(4) -0.2820(3) 0.0333 1.0000 Uani . C1 C -0.1084(2) -0.23571(18) -0.07721(18) 0.0233 1.0000 Uani . C2 C -0.1713(2) -0.27811(19) -0.18835(19) 0.0271 1.0000 Uani . C3 C -0.2258(2) -0.3980(2) -0.2266(2) 0.0332 1.0000 Uani . C4 C -0.2181(2) -0.48284(19) -0.1544(2) 0.0349 1.0000 Uani . C5 C -0.1555(2) -0.44667(19) -0.0458(2) 0.0317 1.0000 Uani . C6 C -0.1032(2) -0.32658(19) -0.0078(2) 0.0278 1.0000 Uani . C7 C 0.2785(3) -0.1421(2) 0.0606(3) 0.0419 1.0000 Uani . C8 C 0.3669(3) -0.1235(2) 0.1739(3) 0.0422 1.0000 Uani . C9 C 0.4522(3) 0.0044(2) 0.1820(3) 0.0412 1.0000 Uani . C10 C 0.3554(3) 0.0641(2) 0.1248(2) 0.0411 1.0000 Uani . C11 C -0.0628(3) 0.3532(3) -0.3358(2) 0.0448 1.0000 Uani . C12 C -0.1531(4) 0.3689(5) -0.4337(3) 0.0773 1.0000 Uani . C13 C -0.1433(5) 0.2816(5) -0.5243(3) 0.0921 1.0000 Uani . C14 C -0.0109(3) 0.2563(3) -0.4924(2) 0.0443 1.0000 Uani . C15 C 0.2370(4) 0.0853(3) -0.4456(3) 0.0614 1.0000 Uani . C16 C 0.3506(4) 0.0679(4) -0.4981(4) 0.0770 1.0000 Uani . C17 C 0.4441(5) 0.1855(4) -0.5005(5) 0.0918 1.0000 Uani . C18 C 0.4011(3) 0.2695(3) -0.4279(3) 0.0619 1.0000 Uani . C19 C 0.4107(2) 0.4780(2) -0.1400(2) 0.0337 1.0000 Uani . C20 C 0.4483(3) 0.6125(2) -0.1283(2) 0.0407 1.0000 Uani . C21 C 0.4041(4) 0.6385(3) -0.2470(3) 0.0560 1.0000 Uani . C22 C 0.2842(4) 0.5356(3) -0.2899(3) 0.0693 1.0000 Uani . F1 F -0.18152(15) -0.20104(12) -0.26421(12) 0.0357 1.0000 Uani . F2 F -0.28828(17) -0.43136(14) -0.33410(14) 0.0490 1.0000 Uani . F3 F -0.27316(17) -0.59976(12) -0.19046(16) 0.0488 1.0000 Uani . F4 F -0.14423(17) -0.52759(12) 0.02644(15) 0.0451 1.0000 Uani . F5 F -0.04322(16) -0.29737(12) 0.09998(12) 0.0375 1.0000 Uani . H71 H 0.3226 -0.1729 0.0006 0.0491 1.0000 Uiso . H72 H 0.1876 -0.1997 0.0629 0.0491 1.0000 Uiso . H81 H 0.4253 -0.1784 0.1765 0.0510 1.0000 Uiso . H82 H 0.3106 -0.1363 0.2362 0.0510 1.0000 Uiso . H91 H 0.5325 0.0119 0.1417 0.0482 1.0000 Uiso . H92 H 0.4840 0.0388 0.2627 0.0482 1.0000 Uiso . H101 H 0.4061 0.1339 0.0890 0.0475 1.0000 Uiso . H102 H 0.3033 0.0913 0.1806 0.0475 1.0000 Uiso . H111 H -0.0230 0.4302 -0.2862 0.0562 1.0000 Uiso . H112 H -0.1140 0.2916 -0.2914 0.0562 1.0000 Uiso . H121 H -0.1221 0.4518 -0.4550 0.0991 1.0000 Uiso . H122 H -0.2486 0.3518 -0.4176 0.0991 1.0000 Uiso . H131 H -0.1451 0.3158 -0.5984 0.1147 1.0000 Uiso . H132 H -0.2203 0.2070 -0.5301 0.1147 1.0000 Uiso . H141 H 0.0531 0.2885 -0.5461 0.0541 1.0000 Uiso . H142 H -0.0255 0.1685 -0.4934 0.0541 1.0000 Uiso . H151 H 0.1531 0.0646 -0.5032 0.0740 1.0000 Uiso . H152 H 0.2209 0.0339 -0.3828 0.0740 1.0000 Uiso . H161 H 0.3175 0.0272 -0.5767 0.0968 1.0000 Uiso . H162 H 0.3971 0.0185 -0.4526 0.0968 1.0000 Uiso . H171 H 0.4397 0.2076 -0.5796 0.1120 1.0000 Uiso . H172 H 0.5391 0.1863 -0.4712 0.1120 1.0000 Uiso . H181 H 0.3947 0.3395 -0.4686 0.0728 1.0000 Uiso . H182 H 0.4680 0.2973 -0.3568 0.0728 1.0000 Uiso . H191 H 0.4903 0.4509 -0.1565 0.0386 1.0000 Uiso . H192 H 0.3813 0.4474 -0.0688 0.0386 1.0000 Uiso . H201 H 0.5483 0.6487 -0.1045 0.0469 1.0000 Uiso . H202 H 0.3981 0.6428 -0.0726 0.0469 1.0000 Uiso . H211 H 0.3790 0.7147 -0.2452 0.0641 1.0000 Uiso . H212 H 0.4776 0.6431 -0.2945 0.0641 1.0000 Uiso . H221 H 0.2787 0.5167 -0.3733 0.0764 1.0000 Uiso . H222 H 0.1994 0.5540 -0.2738 0.0764 1.0000 Uiso . 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 0.02290(11) 0.0193(1) 0.0217(1) 0.00026(7) 0.00468(7) 0.00508(7) Cl1 0.0258(2) 0.0249(2) 0.0348(3) 0.0054(2) 0.0064(2) 0.00314(19) Cl2 0.0357(3) 0.0346(3) 0.0381(3) -0.0108(2) 0.0099(2) 0.0108(2) Cl3 0.0354(3) 0.0335(3) 0.0242(2) 0.0061(2) 0.0003(2) 0.0062(2) N1 0.0227(8) 0.0191(8) 0.0221(8) 0.0010(6) 0.0030(6) 0.0062(6) O1 0.0290(8) 0.0193(7) 0.0335(8) -0.0006(6) -0.0017(6) 0.0087(6) O2 0.0342(9) 0.0383(9) 0.0283(8) -0.0012(7) -0.0013(7) 0.0145(7) O3 0.0357(9) 0.0382(9) 0.041(1) 0.0008(8) 0.0112(8) 0.0105(7) O4 0.046(1) 0.0252(8) 0.041(1) 0.0056(7) -0.0140(8) 0.0053(7) Li1 0.033(2) 0.035(2) 0.031(2) -0.0005(16) -0.0005(16) 0.0113(17) C1 0.0209(9) 0.0197(9) 0.0296(11) 0.0006(8) 0.0064(8) 0.0057(7) C2 0.027(1) 0.024(1) 0.0301(11) -0.0015(8) 0.0034(8) 0.0074(8) C3 0.0312(11) 0.0268(11) 0.0378(13) -0.0095(9) 0.003(1) 0.0062(9) C4 0.0320(12) 0.017(1) 0.0547(15) -0.006(1) 0.0149(11) 0.0034(8) C5 0.0323(11) 0.019(1) 0.0483(14) 0.0069(9) 0.016(1) 0.0096(9) C6 0.027(1) 0.024(1) 0.0334(11) 0.0044(9) 0.0061(9) 0.0079(8) C7 0.0446(14) 0.020(1) 0.0585(17) 0.0079(11) -0.0045(12) 0.009(1) C8 0.0378(13) 0.0329(13) 0.0564(17) 0.0150(12) 0.0015(12) 0.0112(11) C9 0.0373(13) 0.0343(13) 0.0489(15) 0.0076(11) -0.0059(11) 0.0101(11) C10 0.0483(15) 0.0251(11) 0.0454(15) -0.005(1) -0.0146(12) 0.0148(11) C11 0.0460(15) 0.0600(17) 0.0347(14) -0.0018(12) 0.0014(11) 0.0293(14) C12 0.075(2) 0.128(4) 0.0454(19) -0.014(2) -0.0080(17) 0.069(3) C13 0.084(3) 0.146(4) 0.057(2) -0.047(3) -0.029(2) 0.082(3) C14 0.0490(15) 0.0568(17) 0.0296(13) -0.0092(12) -0.0026(11) 0.0265(13) C15 0.077(2) 0.0413(16) 0.066(2) -0.0086(15) 0.0380(18) 0.0097(15) C16 0.066(2) 0.071(2) 0.105(3) -0.012(2) 0.029(2) 0.034(2) C17 0.068(3) 0.092(3) 0.121(4) -0.005(3) 0.058(3) 0.016(2) C18 0.0436(17) 0.0564(19) 0.082(2) 0.0022(17) 0.0259(17) 0.0022(14) C19 0.0308(11) 0.0274(11) 0.0382(13) 0.0046(9) -0.004(1) 0.0044(9) C20 0.0416(14) 0.0266(12) 0.0491(15) 0.0036(11) 0.0017(12) 0.004(1) C21 0.066(2) 0.0349(14) 0.060(2) 0.0145(13) -0.0104(16) 0.0084(14) C22 0.084(3) 0.0354(15) 0.071(2) 0.0187(15) -0.0323(19) 0.0049(15) F1 0.0473(8) 0.0298(7) 0.0274(7) -0.0007(5) -0.0035(6) 0.0120(6) F2 0.055(1) 0.0381(8) 0.0432(9) -0.0196(7) -0.0051(7) 0.0079(7) F3 0.0484(9) 0.0178(6) 0.0753(12) -0.0110(7) 0.0186(8) 0.0014(6) F4 0.0509(9) 0.0240(7) 0.0677(11) 0.0188(7) 0.0207(8) 0.0142(6) F5 0.0459(8) 0.0302(7) 0.0348(8) 0.0095(6) -0.0003(6) 0.0098(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zr1 . Cl1 . 2.5497(5) yes Zr1 . Cl2 . 2.4871(6) yes Zr1 . Cl3 . 2.4674(6) yes Zr1 . N1 . 2.0892(17) yes Zr1 . N1 2_555 2.1229(17) yes Zr1 . O1 . 2.2778(15) yes Cl1 . Li1 . 2.570(4) yes Cl3 . Li1 . 2.785(4) yes N1 . C1 . 1.384(3) yes O1 . C7 . 1.459(3) yes O1 . C10 . 1.457(3) yes O2 . Li1 . 1.996(4) yes O2 . C11 . 1.442(3) yes O2 . C14 . 1.441(3) yes O3 . Li1 . 1.963(5) yes O3 . C15 . 1.437(3) yes O3 . C18 . 1.417(3) yes O4 . Li1 . 2.007(4) yes O4 . C19 . 1.433(3) yes O4 . C22 . 1.440(3) yes Li1 . F5 2_555 2.843(5) yes C1 . C2 . 1.399(3) yes C1 . C6 . 1.408(3) yes C2 . C3 . 1.386(3) yes C2 . F1 . 1.343(3) yes C3 . C4 . 1.378(4) yes C3 . F2 . 1.346(3) yes C4 . C5 . 1.362(4) yes C4 . F3 . 1.350(2) yes C5 . C6 . 1.385(3) yes C5 . F4 . 1.349(3) yes C6 . F5 . 1.339(3) yes C7 . C8 . 1.505(4) yes C8 . C9 . 1.507(3) yes C9 . C10 . 1.501(3) yes C11 . C12 . 1.462(4) yes C12 . C13 . 1.475(5) yes C13 . C14 . 1.493(4) yes C15 . C16 . 1.458(4) yes C16 . C17 . 1.456(6) yes C17 . C18 . 1.469(5) yes C19 . C20 . 1.512(3) yes C20 . C21 . 1.517(4) yes C21 . C22 . 1.480(4) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Zr1 . Cl2 . 96.07(2) yes Cl1 . Zr1 . Cl3 . 85.967(19) yes Cl2 . Zr1 . Cl3 . 92.22(2) yes Cl1 . Zr1 . N1 . 169.87(5) yes Cl2 . Zr1 . N1 . 92.07(5) yes Cl3 . Zr1 . N1 . 99.76(5) yes Cl1 . Zr1 . N1 2_555 91.35(5) yes Cl2 . Zr1 . N1 2_555 166.19(5) yes Cl3 . Zr1 . N1 2_555 99.93(5) yes N1 . Zr1 . N1 2_555 79.48(7) yes Cl1 . Zr1 . O1 . 82.26(4) yes Cl2 . Zr1 . O1 . 81.18(4) yes Cl3 . Zr1 . O1 . 165.79(4) yes N1 . Zr1 . O1 . 93.08(6) yes N1 2_555 Zr1 . O1 . 88.33(6) yes Zr1 . Cl1 . Li1 . 98.9(1) yes Zr1 . Cl3 . Li1 . 95.38(9) yes Zr1 . N1 . Zr1 2_555 100.52(7) yes Zr1 . N1 . C1 . 128.37(13) yes Zr1 2_555 N1 . C1 . 131.07(14) yes Zr1 . O1 . C7 . 126.22(14) yes Zr1 . O1 . C10 . 124.52(13) yes C7 . O1 . C10 . 108.74(18) yes Li1 . O2 . C11 . 123.05(19) yes Li1 . O2 . C14 . 121.40(19) yes C11 . O2 . C14 . 107.62(19) yes Li1 . O3 . C15 . 123.6(2) yes Li1 . O3 . C18 . 124.0(2) yes C15 . O3 . C18 . 109.3(2) yes Li1 . O4 . C19 . 128.10(18) yes Li1 . O4 . C22 . 122.8(2) yes C19 . O4 . C22 . 109.1(2) yes Cl1 . Li1 . O2 . 161.1(2) yes Cl3 . Li1 . O2 . 85.70(15) yes Cl1 . Li1 . O3 . 95.77(17) yes Cl3 . Li1 . O3 . 101.86(17) yes O2 . Li1 . O3 . 98.5(2) yes Cl1 . Li1 . O4 . 93.46(16) yes Cl3 . Li1 . O4 . 152.1(2) yes O2 . Li1 . O4 . 94.48(19) yes O3 . Li1 . O4 . 105.7(2) yes Cl1 . Li1 . F5 2_555 76.87(12) yes Cl3 . Li1 . F5 2_555 66.1(1) yes O2 . Li1 . F5 2_555 86.61(15) yes O3 . Li1 . F5 2_555 166.7(2) yes O4 . Li1 . F5 2_555 85.97(15) yes N1 . C1 . C2 . 123.42(19) yes N1 . C1 . C6 . 122.9(2) yes C2 . C1 . C6 . 113.65(19) yes C1 . C2 . C3 . 123.5(2) yes C1 . C2 . F1 . 119.99(19) yes C3 . C2 . F1 . 116.5(2) yes C2 . C3 . C4 . 120.1(2) yes C2 . C3 . F2 . 119.8(2) yes C4 . C3 . F2 . 120.1(2) yes C3 . C4 . C5 . 118.9(2) yes C3 . C4 . F3 . 120.5(2) yes C5 . C4 . F3 . 120.6(2) yes C4 . C5 . C6 . 120.5(2) yes C4 . C5 . F4 . 120.3(2) yes C6 . C5 . F4 . 119.1(2) yes C1 . C6 . C5 . 123.3(2) yes C1 . C6 . F5 . 119.35(19) yes C5 . C6 . F5 . 117.4(2) yes O1 . C7 . C8 . 106.0(2) yes C7 . C8 . C9 . 103.4(2) yes C8 . C9 . C10 . 102.9(2) yes O1 . C10 . C9 . 105.97(19) yes O2 . C11 . C12 . 106.4(2) yes C11 . C12 . C13 . 104.4(3) yes C12 . C13 . C14 . 106.3(3) yes O2 . C14 . C13 . 106.6(2) yes O3 . C15 . C16 . 107.8(3) yes C15 . C16 . C17 . 106.9(3) yes C16 . C17 . C18 . 107.0(3) yes O3 . C18 . C17 . 107.6(3) yes O4 . C19 . C20 . 106.73(19) yes C19 . C20 . C21 . 102.7(2) yes C20 . C21 . C22 . 103.5(2) yes O4 . C22 . C21 . 107.3(2) yes #===end data_COMPOUND_9 _database_code_depnum_ccdc_archive 'CCDC 260436' # Local Code SE1 _chemical_name_systematic ; [Zr2(mu-N-2,6-C6H3Me2)2Cl4(NHMe2)2(THF)2] ; _chemical_name_common (Zr2(mu-N-2,6-C6H3Me2)2Cl4(NHMe2)2(THF)2) _publ_section_exptl_refinement ; no special requirements ; _cell_length_a 21.140(1) _cell_angle_alpha 90 _cell_length_b 9.467(1) _cell_angle_beta 90 _cell_length_c 17.084(1) _cell_angle_gamma 90 _cell_volume 3419.1(4) _symmetry_cell_setting 'Orthorhombic ' _symmetry_space_group_name_H-M 'P c a 21 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x+1/2,y,z+1/2 x+1/2,-y,z -x,-y,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'Zr ' -2.9650 0.5600 17.8765 1.2762 10.9480 11.9160 5.4173 0.1176 3.6572 87.6627 2.0693 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 4 _chemical_formula_sum ' C28 H48 Cl4 N4 O2 Zr2 ' _chemical_formula_moiety ' C28 H48 Cl4 N4 O2 Zr2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 796.97 _cell_measurement_reflns_used 7313 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _cell_measurement_temperature 150 #_cell_formula_units_Z 4 _exptl_crystal_description ' block ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.24 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.55 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method none _exptl_crystal_F_000 1610.32 _exptl_absorpt_coefficient_mu 0.95 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.766 _exptl_absorpt_correction_T_max 0.796 _diffrn_standards_interval_time 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method CCD _diffrn_ambient_temperature 150 _diffrn_reflns_number 14507 _reflns_number_total 7793 _diffrn_reflns_av_R_equivalents 0.02 _reflns_number_gt 7027 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min 0 _reflns_limit_h_max 27 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min -22 _reflns_limit_l_max 22 _refine_diff_density_min -0.68 _refine_diff_density_max 0.71 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 7027 _refine_ls_number_parameters 362 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0267 _refine_ls_goodness_of_fit_ref 1.0185 _refine_ls_shift/su_max 0.0007 _refine_ls_abs_structure_Flack -0.01(6) _refine_ls_structure_factor_coef F _refine_ls_hydrogen_treatment 'riding model' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_hydrogens geometric _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 0.693 0.734E-010.445 ; _refine_ls_extinction_coef 112.3(140) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Zr1 -0.12339(1) 0.36914(2) 0.51771(3) 0.0191 1.0000 Uani Zr2 -0.098560(9) 0.11368(2) 0.40446(3) 0.0188 1.0000 Uani Cl1 -0.16380(3) 0.56233(6) 0.43207(4) 0.0277 1.0000 Uani Cl2 -0.08763(3) 0.28406(7) 0.64635(4) 0.0309 1.0000 Uani Cl3 -0.12995(3) 0.19976(7) 0.27417(4) 0.0279 1.0000 Uani Cl4 -0.06291(3) -0.07842(6) 0.49479(4) 0.0302 1.0000 Uani N1 -0.0517(1) 0.2940(2) 0.45182(12) 0.0210 1.0000 Uani N2 -0.17022(9) 0.1873(2) 0.46862(12) 0.0212 1.0000 Uani N3 -0.05980(12) 0.5733(2) 0.55841(13) 0.0310 1.0000 Uani N4 -0.15637(12) -0.0958(2) 0.35715(14) 0.0306 1.0000 Uani O1 -0.21247(9) 0.44569(19) 0.5946(1) 0.0265 1.0000 Uani O2 -0.00694(9) 0.0382(2) 0.33505(12) 0.0314 1.0000 Uani C1 0.01241(11) 0.3233(2) 0.43143(16) 0.0235 1.0000 Uani C2 0.06246(13) 0.2624(3) 0.47509(16) 0.0289 1.0000 Uani C3 0.12484(13) 0.2881(3) 0.4515(2) 0.0376 1.0000 Uani C4 0.13876(14) 0.3745(3) 0.3898(2) 0.0439 1.0000 Uani C5 0.09009(14) 0.4403(3) 0.34962(19) 0.0389 1.0000 Uani C6 0.02656(13) 0.4164(3) 0.36910(15) 0.0271 1.0000 Uani C7 0.05117(13) 0.1785(3) 0.54824(19) 0.0374 1.0000 Uani C8 -0.02452(15) 0.4933(3) 0.32471(18) 0.0365 1.0000 Uani C9 -0.23424(11) 0.1713(2) 0.49249(14) 0.0199 1.0000 Uani C10 -0.28395(12) 0.2321(3) 0.44828(14) 0.0240 1.0000 Uani C11 -0.34578(13) 0.2246(3) 0.47549(16) 0.0314 1.0000 Uani C12 -0.36039(13) 0.1528(3) 0.54366(18) 0.0358 1.0000 Uani C13 -0.31266(13) 0.0846(3) 0.58419(16) 0.0309 1.0000 Uani C14 -0.24985(12) 0.0918(3) 0.56002(15) 0.0250 1.0000 Uani C15 -0.27150(12) 0.3000(3) 0.37015(15) 0.0277 1.0000 Uani C16 -0.20073(14) 0.0123(3) 0.60490(17) 0.0374 1.0000 Uani C17 0.00770(15) 0.5577(3) 0.5803(2) 0.0414 1.0000 Uani C18 -0.09328(16) 0.6514(3) 0.62121(18) 0.0382 1.0000 Uani C19 -0.26557(14) 0.5310(3) 0.56546(17) 0.0322 1.0000 Uani C20 -0.31564(15) 0.5237(4) 0.62930(19) 0.0430 1.0000 Uani C21 -0.27594(15) 0.5128(3) 0.70273(16) 0.0366 1.0000 Uani C22 -0.22552(15) 0.4106(3) 0.67696(16) 0.0331 1.0000 Uani C23 -0.12531(14) -0.1681(3) 0.29123(18) 0.0367 1.0000 Uani C24 -0.22466(15) -0.0797(3) 0.3411(2) 0.0428 1.0000 Uani C25 0.04269(16) -0.0549(4) 0.3652(2) 0.0524 1.0000 Uani C26 0.09901(17) -0.0393(4) 0.3159(2) 0.0507 1.0000 Uani C27 0.08418(17) 0.0753(4) 0.2586(2) 0.0495 1.0000 Uani C28 0.01298(16) 0.0848(4) 0.2581(2) 0.0514 1.0000 Uani H1 -0.05671 0.6190 0.51440 0.0387 1.0000 Uiso H2 -0.15446 -0.1505 0.39801 0.0398 1.0000 Uiso H31 0.16031 0.2413 0.4802 0.0450 1.0000 Uiso H41 0.18360 0.3920 0.3738 0.0521 1.0000 Uiso H51 0.10015 0.5053 0.30516 0.0445 1.0000 Uiso H71 0.09229 0.1441 0.56999 0.0446 1.0000 Uiso H72 0.02983 0.2404 0.58764 0.0446 1.0000 Uiso H73 0.02337 0.0959 0.53603 0.0446 1.0000 Uiso H81 -0.00499 0.5536 0.28318 0.0423 1.0000 Uiso H82 -0.04899 0.5541 0.36175 0.0423 1.0000 Uiso H83 -0.05360 0.4230 0.29994 0.0423 1.0000 Uiso H111 -0.38039 0.2714 0.44515 0.0357 1.0000 Uiso H121 -0.40480 0.1506 0.56381 0.0411 1.0000 Uiso H131 -0.32348 0.0279 0.63176 0.0363 1.0000 Uiso H151 -0.31194 0.3367 0.34765 0.0341 1.0000 Uiso H152 -0.24107 0.3798 0.37725 0.0341 1.0000 Uiso H153 -0.25286 0.2285 0.33374 0.0341 1.0000 Uiso H161 -0.22097 -0.0371 0.65016 0.0466 1.0000 Uiso H162 -0.16801 0.0798 0.62470 0.0466 1.0000 Uiso H163 -0.18027 -0.0588 0.56980 0.0466 1.0000 Uiso H171 0.03036 0.5052 0.5379 0.0506 1.0000 Uiso H172 0.02754 0.6527 0.5874 0.0506 1.0000 Uiso H173 0.01068 0.5034 0.6304 0.0506 1.0000 Uiso H181 -0.13879 0.6634 0.60668 0.0446 1.0000 Uiso H182 -0.07333 0.7463 0.62821 0.0446 1.0000 Uiso H183 -0.09020 0.5969 0.67123 0.0446 1.0000 Uiso H191 -0.25184 0.6309 0.55705 0.0398 1.0000 Uiso H192 -0.28190 0.4912 0.51514 0.0398 1.0000 Uiso H201 -0.34268 0.6104 0.62973 0.0520 1.0000 Uiso H202 -0.34300 0.4384 0.62274 0.0520 1.0000 Uiso H211 -0.30079 0.4749 0.74791 0.0418 1.0000 Uiso H212 -0.25740 0.6064 0.71717 0.0418 1.0000 Uiso H221 -0.18636 0.4224 0.70914 0.0406 1.0000 Uiso H222 -0.24110 0.3113 0.68170 0.0406 1.0000 Uiso H231 -0.07922 -0.1796 0.30279 0.0435 1.0000 Uiso H232 -0.14498 -0.2631 0.28334 0.0435 1.0000 Uiso H233 -0.13063 -0.1103 0.24267 0.0435 1.0000 Uiso H241 -0.24499 -0.0308 0.3865 0.0498 1.0000 Uiso H242 -0.24475 -0.1743 0.3334 0.0498 1.0000 Uiso H243 -0.23041 -0.0215 0.2928 0.0498 1.0000 Uiso H251 0.05322 -0.0288 0.4204 0.0687 1.0000 Uiso H252 0.02752 -0.1549 0.3635 0.0687 1.0000 Uiso H261 0.13656 -0.0137 0.3486 0.0597 1.0000 Uiso H262 0.10773 -0.1293 0.2872 0.0597 1.0000 Uiso H271 0.10239 0.1669 0.2771 0.0602 1.0000 Uiso H272 0.10138 0.0524 0.2056 0.0602 1.0000 Uiso H281 -0.00183 0.1831 0.2472 0.0620 1.0000 Uiso H282 -0.00442 0.0192 0.2175 0.0620 1.0000 Uiso 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 0.0203(1) 0.01836(9) 0.0186(1) 0.00227(8) -0.00060(8) -0.00038(8) Zr2 0.0189(1) 0.01738(9) 0.0200(1) 0.00202(9) -0.00170(8) -0.00092(8) Cl1 0.0339(3) 0.0227(3) 0.0265(3) 0.0070(2) -0.0024(2) 0.0018(2) Cl2 0.0342(3) 0.0335(3) 0.0250(3) 0.0066(2) -0.0053(2) 0.0021(2) Cl3 0.0328(3) 0.0292(3) 0.0216(3) 0.0043(2) -0.0044(2) 0.0018(2) Cl4 0.0323(3) 0.0238(3) 0.0344(3) 0.0089(2) -0.0060(3) 0.0007(2) N1 0.0187(9) 0.0213(9) 0.023(1) 0.0039(7) -0.0001(7) -0.0044(8) N2 0.0167(9) 0.0220(9) 0.025(1) 0.0065(8) -0.0021(7) -0.0018(7) N3 0.0400(13) 0.0279(11) 0.0250(11) 0.0008(9) -0.0030(9) -0.0078(9) N4 0.0376(12) 0.024(1) 0.0305(12) 0.0050(8) -0.008(1) -0.0043(9) O1 0.0288(9) 0.0287(9) 0.0221(9) -0.0010(7) 0.0013(7) 0.0036(7) O2 0.030(1) 0.032(1) 0.032(1) 0.0009(8) 0.0009(8) 0.0030(8) C1 0.0213(11) 0.018(1) 0.0308(12) -0.0079(9) 0.0031(9) -0.0038(9) C2 0.0198(12) 0.0245(12) 0.0424(16) -0.0109(11) -0.005(1) -0.0043(9) C3 0.0209(13) 0.0402(15) 0.0519(18) -0.0187(13) -0.0005(12) -0.0033(11) C4 0.0228(12) 0.0524(18) 0.057(2) -0.0193(15) 0.0126(13) -0.0100(12) C5 0.0364(15) 0.0429(16) 0.0374(15) -0.0106(12) 0.0160(13) -0.0155(12) C6 0.0285(13) 0.0255(12) 0.0274(12) -0.006(1) 0.008(1) -0.010(1) C7 0.0259(14) 0.0344(15) 0.0520(17) 0.0037(13) -0.0135(12) 0.0020(11) C8 0.0405(16) 0.0335(14) 0.0354(15) 0.0092(12) 0.0080(12) -0.0074(12) C9 0.018(1) 0.019(1) 0.0234(11) -0.0020(8) -0.0000(8) -0.0042(8) C10 0.0216(12) 0.0238(11) 0.0267(13) -0.0024(9) -0.0030(9) 0.0003(9) C11 0.0209(12) 0.0310(13) 0.0424(16) -0.0039(11) 0.0004(11) 0.003(1) C12 0.0217(12) 0.0389(14) 0.0469(16) -0.0054(12) 0.0109(11) -0.0039(11) C13 0.0301(13) 0.0326(13) 0.0299(13) -0.0010(11) 0.007(1) -0.0106(11) C14 0.0246(12) 0.0250(12) 0.0254(12) 0.0003(9) 0.0000(9) -0.007(1) C15 0.0217(12) 0.0313(13) 0.0300(13) 0.006(1) -0.006(1) 0.001(1) C16 0.0326(14) 0.0421(15) 0.0375(15) 0.0210(13) 0.0003(12) -0.0078(12) C17 0.0378(16) 0.0368(15) 0.0497(19) -0.0054(13) -0.0088(14) -0.0086(12) C18 0.0561(19) 0.0250(12) 0.0336(15) -0.0031(11) 0.0003(13) -0.0030(12) C19 0.0329(14) 0.0334(14) 0.0304(14) -0.0008(11) -0.0036(11) 0.0097(11) C20 0.0343(15) 0.0542(18) 0.0405(16) 0.0016(14) 0.0086(13) 0.0111(14) C21 0.0419(16) 0.0407(15) 0.0272(13) 0.0014(11) 0.0103(12) 0.0065(12) C22 0.0369(14) 0.0373(14) 0.0250(13) 0.0060(11) 0.0105(11) 0.0027(12) C23 0.0426(16) 0.0262(13) 0.0412(16) -0.0036(12) -0.0045(12) -0.0016(12) C24 0.0369(16) 0.0385(16) 0.0532(19) -0.0097(14) -0.0044(14) -0.0104(12) C25 0.0321(16) 0.058(2) 0.067(2) 0.0175(18) 0.0055(15) 0.0184(15) C26 0.0437(18) 0.063(2) 0.0454(18) 0.0012(16) 0.0047(15) 0.0184(16) C27 0.0457(18) 0.0506(18) 0.052(2) 0.0056(16) 0.0206(15) 0.0126(15) C28 0.0382(17) 0.074(2) 0.0419(18) 0.0180(17) 0.0126(14) 0.0144(17) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zr1 . Zr2 . 3.1414(3) yes Zr1 . Cl1 . 2.4931(6) yes Zr1 . Cl2 . 2.4596(7) yes Zr1 . N1 . 2.017(2) yes Zr1 . N2 . 2.156(2) yes Zr1 . N3 . 2.455(2) yes Zr1 . O1 . 2.4073(18) yes Zr2 . Cl3 . 2.4615(6) yes Zr2 . Cl4 . 2.5014(6) yes Zr2 . N1 . 2.133(2) yes Zr2 . N2 . 1.996(2) yes Zr2 . N4 . 2.466(2) yes Zr2 . O2 . 2.381(2) yes N1 . C1 . 1.427(3) yes N2 . C9 . 1.422(3) yes N3 . C17 . 1.483(4) yes N3 . C18 . 1.483(4) yes N4 . C23 . 1.472(4) yes N4 . C24 . 1.477(4) yes O1 . C19 . 1.470(3) yes O1 . C22 . 1.472(3) yes O2 . C25 . 1.464(4) yes O2 . C28 . 1.449(4) yes C1 . C2 . 1.417(4) yes C1 . C6 . 1.414(4) yes C2 . C3 . 1.400(4) yes C2 . C7 . 1.500(4) yes C3 . C4 . 1.366(5) yes C4 . C5 . 1.385(5) yes C5 . C6 . 1.402(4) yes C6 . C8 . 1.507(4) yes C9 . C10 . 1.416(3) yes C9 . C14 . 1.416(3) yes C10 . C11 . 1.389(4) yes C10 . C15 . 1.505(4) yes C11 . C12 . 1.383(4) yes C12 . C13 . 1.384(4) yes C13 . C14 . 1.392(4) yes C14 . C16 . 1.494(4) yes C19 . C20 . 1.521(4) yes C20 . C21 . 1.513(4) yes C21 . C22 . 1.505(4) yes C25 . C26 . 1.466(5) yes C26 . C27 . 1.494(5) yes C27 . C28 . 1.508(5) yes Cl1 . H2 1_565 2.787(2) no Cl4 . H1 1_545 2.887(2) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Zr2 . Zr1 . Cl1 . 105.106(17) yes Zr2 . Zr1 . Cl2 . 104.286(17) yes Cl1 . Zr1 . Cl2 . 150.45(2) yes Zr2 . Zr1 . N1 . 42.19(6) yes Cl1 . Zr1 . N1 . 100.87(6) yes Cl2 . Zr1 . N1 . 98.76(6) yes Zr2 . Zr1 . N2 . 38.95(5) yes Cl1 . Zr1 . N2 . 101.54(5) yes Cl2 . Zr1 . N2 . 103.14(5) yes N1 . Zr1 . N2 . 81.14(8) yes Zr2 . Zr1 . N3 . 133.56(6) yes Cl1 . Zr1 . N3 . 77.07(6) yes Cl2 . Zr1 . N3 . 80.58(6) yes N1 . Zr1 . N3 . 91.41(8) yes N2 . Zr1 . N3 . 172.07(8) yes Zr2 . Zr1 . O1 . 134.30(4) yes Cl1 . Zr1 . O1 . 80.28(4) yes Cl2 . Zr1 . O1 . 81.47(5) yes N1 . Zr1 . O1 . 176.46(7) yes N2 . Zr1 . O1 . 95.36(7) yes N3 . Zr1 . O1 . 92.11(7) yes Zr1 . Zr2 . Cl3 . 104.892(17) yes Zr1 . Zr2 . Cl4 . 103.306(18) yes Cl3 . Zr2 . Cl4 . 151.62(2) yes Zr1 . Zr2 . N1 . 39.43(6) yes Cl3 . Zr2 . N1 . 101.72(5) yes Cl4 . Zr2 . N1 . 102.01(6) yes Zr1 . Zr2 . N2 . 42.77(6) yes Cl3 . Zr2 . N2 . 100.16(6) yes Cl4 . Zr2 . N2 . 98.27(6) yes N1 . Zr2 . N2 . 82.20(8) yes Zr1 . Zr2 . N4 . 137.59(6) yes Cl3 . Zr2 . N4 . 80.58(6) yes Cl4 . Zr2 . N4 . 76.51(5) yes N1 . Zr2 . N4 . 176.52(8) yes N2 . Zr2 . N4 . 94.86(8) yes Zr1 . Zr2 . O2 . 132.37(5) yes Cl3 . Zr2 . O2 . 82.43(5) yes Cl4 . Zr2 . O2 . 81.02(5) yes N1 . Zr2 . O2 . 92.97(7) yes N2 . Zr2 . O2 . 174.88(8) yes N4 . Zr2 . O2 . 89.91(8) yes Zr1 . N1 . Zr2 . 98.38(8) yes Zr1 . N1 . C1 . 141.37(16) yes Zr2 . N1 . C1 . 120.25(15) yes Zr1 . N2 . Zr2 . 98.28(8) yes Zr1 . N2 . C9 . 114.26(15) yes Zr2 . N2 . C9 . 147.45(16) yes Zr1 . N3 . C17 . 121.35(18) yes Zr1 . N3 . C18 . 109.64(17) yes C17 . N3 . C18 . 109.1(2) yes Zr2 . N4 . C23 . 113.79(17) yes Zr2 . N4 . C24 . 117.50(17) yes C23 . N4 . C24 . 110.0(2) yes Zr1 . O1 . C19 . 125.33(15) yes Zr1 . O1 . C22 . 126.88(16) yes C19 . O1 . C22 . 107.7(2) yes Zr2 . O2 . C25 . 126.0(2) yes Zr2 . O2 . C28 . 126.65(18) yes C25 . O2 . C28 . 107.1(2) yes N1 . C1 . C2 . 120.1(2) yes N1 . C1 . C6 . 120.4(2) yes C2 . C1 . C6 . 119.5(2) yes C1 . C2 . C3 . 118.7(3) yes C1 . C2 . C7 . 122.4(2) yes C3 . C2 . C7 . 118.8(3) yes C2 . C3 . C4 . 122.0(3) yes C3 . C4 . C5 . 119.4(3) yes C4 . C5 . C6 . 121.4(3) yes C1 . C6 . C5 . 118.8(3) yes C1 . C6 . C8 . 121.9(2) yes C5 . C6 . C8 . 119.3(3) yes N2 . C9 . C10 . 120.7(2) yes N2 . C9 . C14 . 120.8(2) yes C10 . C9 . C14 . 118.5(2) yes C9 . C10 . C11 . 119.9(2) yes C9 . C10 . C15 . 121.1(2) yes C11 . C10 . C15 . 118.9(2) yes C10 . C11 . C12 . 121.1(3) yes C11 . C12 . C13 . 119.2(2) yes C12 . C13 . C14 . 121.6(3) yes C9 . C14 . C13 . 119.3(2) yes C9 . C14 . C16 . 121.6(2) yes C13 . C14 . C16 . 119.1(2) yes O1 . C19 . C20 . 105.3(2) yes C19 . C20 . C21 . 102.2(2) yes C20 . C21 . C22 . 101.2(2) yes O1 . C22 . C21 . 105.5(2) yes O2 . C25 . C26 . 108.6(3) yes C25 . C26 . C27 . 106.2(3) yes C26 . C27 . C28 . 104.9(3) yes O2 . C28 . C27 . 105.4(3) yes Cl4 1_565 H1 . N3 . 126.19(5) no Cl1 1_545 H2 . N4 . 138.14(5) no #===end data_COMPOUND_12 _database_code_depnum_ccdc_archive 'CCDC 260437' # Local code SRD10 _chemical_name_systematic ; [ZrCl2(NHMe2)(mu-N-t-Bu)2ZrCl2(NHMe2)2] ; _chemical_name_common (ZrCl2(NHMe2)(mu-N-t-Bu)2ZrCl2(NHMe2)2) _publ_section_exptl_refinement ; no special comment ; _cell_length_a 10.0181(1) _cell_length_b 10.0274(1) _cell_length_c 14.3986(2) _cell_angle_alpha 97.5478(6) _cell_angle_beta 101.1935(6) _cell_angle_gamma 110.7356(6) _cell_volume 1295.05(3) _symmetry_cell_setting 'Triclinic ' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'Zr ' -2.9650 0.5600 17.8765 1.2762 10.9480 11.9160 5.4173 0.1176 3.6572 87.6627 2.0693 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum ' C14 H39 Cl4 N5 Zr2 ' _chemical_formula_moiety ' C14 H39 Cl4 N5 Zr2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 601.75 _cell_measurement_reflns_used 5518 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description ' block ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.32 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.54 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method none _exptl_crystal_F_000 601.10 _exptl_absorpt_coefficient_mu 1.23 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.658 _exptl_absorpt_correction_T_max 0.675 _diffrn_standards_interval_time 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method CCD _diffrn_ambient_temperature 150 _diffrn_reflns_number 11080 _reflns_number_total 5912 _diffrn_reflns_av_R_equivalents 0.01 _reflns_number_gt 5263 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.52 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min -13 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _refine_diff_density_min -0.39 _refine_diff_density_max 0.42 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 5263 _refine_ls_number_parameters 227 _refine_ls_R_factor_gt 0.0194 _refine_ls_wR_factor_ref 0.0093 _refine_ls_goodness_of_fit_ref 1.0588 _refine_ls_shift/su_max 0.002660 _refine_ls_structure_factor_coef F _refine_ls_hydrogen_treatment 'riding model' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_hydrogens geometric _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_abs_structure_flack none _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 4 parameters, Carruthers & Watkin , 1979, 0.222 -.748 -.118 -.364 ; _refine_ls_extinction_coef 75(34) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SIR92 (Altomare, et al., 1994)' _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin et al., 1996) ; _computing_molecular_graphics 'CAMERON (Watkin, Prout and Pearce, 1996)' _computing_publication_material ; CRYSTALS Issue 10 (Watkin et al., 1996) ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Zr1 0.353374(14) 0.564370(13) 0.731469(9) 0.0137 1.0000 Uani Zr2 0.084929(13) 0.312675(13) 0.758468(9) 0.0136 1.0000 Uani Cl1 0.51267(4) 0.67102(4) 0.90097(2) 0.0261 1.0000 Uani Cl2 0.26926(4) 0.55540(4) 0.55518(2) 0.0262 1.0000 Uani Cl3 -0.13867(4) 0.29718(4) 0.81860(3) 0.0227 1.0000 Uani Cl4 0.00196(4) 0.03675(4) 0.72121(3) 0.0225 1.0000 Uani N1 0.29070(12) 0.35019(12) 0.73083(8) 0.0158 1.0000 Uani N2 0.15762(12) 0.53476(12) 0.76202(8) 0.0151 1.0000 Uani N3 0.58123(13) 0.75035(13) 0.70992(9) 0.0235 1.0000 Uani N4 -0.06189(14) 0.26230(13) 0.59552(8) 0.0215 1.0000 Uani N5 0.18407(13) 0.31551(13) 0.92332(8) 0.0208 1.0000 Uani C1 0.39901(15) 0.28175(14) 0.7236(1) 0.0187 1.0000 Uani C2 0.33435(17) 0.15228(16) 0.63635(11) 0.0261 1.0000 Uani C3 0.43828(17) 0.23123(17) 0.81697(11) 0.0263 1.0000 Uani C4 0.53947(16) 0.39373(16) 0.70876(12) 0.0258 1.0000 Uani C5 0.10692(15) 0.65786(14) 0.7686(1) 0.0188 1.0000 Uani C6 -0.03501(17) 0.61705(17) 0.68969(13) 0.0295 1.0000 Uani C7 0.0819(2) 0.69316(18) 0.86849(13) 0.0337 1.0000 Uani C8 0.22614(16) 0.79500(15) 0.75478(12) 0.0245 1.0000 Uani C9 0.62562(18) 0.73300(18) 0.61801(12) 0.0331 1.0000 Uani C10 0.5928(2) 0.90223(17) 0.73841(15) 0.0384 1.0000 Uani C11 -0.00454(17) 0.19651(17) 0.52266(11) 0.0277 1.0000 Uani C12 -0.22268(17) 0.17643(19) 0.57602(12) 0.0308 1.0000 Uani C13 0.10953(18) 0.18407(17) 0.95979(11) 0.0295 1.0000 Uani C14 0.20001(17) 0.44868(17) 0.9903(1) 0.0253 1.0000 Uani H3 0.64512 0.73121 0.75034 0.0195 1.0000 Uiso H4 -0.05271 0.35015 0.58963 0.0175 1.0000 Uiso H5 0.27059 0.31505 0.92274 0.0182 1.0000 Uiso H21 0.40779 0.10688 0.63199 0.0320 1.0000 Uiso H22 0.24185 0.07817 0.64431 0.0320 1.0000 Uiso H23 0.31106 0.18732 0.57571 0.0320 1.0000 Uiso H31 0.51105 0.18518 0.81195 0.0350 1.0000 Uiso H32 0.48264 0.31722 0.87309 0.0350 1.0000 Uiso H33 0.34682 0.15832 0.82702 0.0350 1.0000 Uiso H41 0.61250 0.34799 0.70381 0.0336 1.0000 Uiso H42 0.58337 0.47942 0.76506 0.0336 1.0000 Uiso H43 0.51404 0.42705 0.64770 0.0336 1.0000 Uiso H61 -0.06903 0.69961 0.69407 0.0353 1.0000 Uiso H62 -0.11312 0.52778 0.69832 0.0353 1.0000 Uiso H63 -0.01592 0.59683 0.62471 0.0353 1.0000 Uiso H71 0.0481 0.77586 0.87240 0.0473 1.0000 Uiso H72 0.1768 0.72157 0.91912 0.0473 1.0000 Uiso H73 0.0051 0.60521 0.87962 0.0473 1.0000 Uiso H81 0.19197 0.87746 0.75929 0.0295 1.0000 Uiso H82 0.31955 0.82215 0.80648 0.0295 1.0000 Uiso H83 0.24466 0.77464 0.68963 0.0295 1.0000 Uiso H91 0.61890 0.63088 0.59857 0.0385 1.0000 Uiso H92 0.72942 0.80337 0.62703 0.0385 1.0000 Uiso H93 0.55766 0.75310 0.56621 0.0385 1.0000 Uiso H101 0.5638 0.91512 0.80062 0.0469 1.0000 Uiso H102 0.6967 0.97211 0.74708 0.0469 1.0000 Uiso H103 0.5249 0.92184 0.68626 0.0469 1.0000 Uiso H111 0.10394 0.25391 0.53477 0.0314 1.0000 Uiso H112 -0.02233 0.09358 0.52817 0.0314 1.0000 Uiso H113 -0.05648 0.19699 0.45605 0.0314 1.0000 Uiso H121 -0.26309 0.22025 0.62454 0.0347 1.0000 Uiso H122 -0.23960 0.07359 0.58132 0.0347 1.0000 Uiso H123 -0.27375 0.17700 0.50919 0.0347 1.0000 Uiso H131 0.09937 0.09425 0.91462 0.0362 1.0000 Uiso H132 0.16937 0.19079 1.02577 0.0362 1.0000 Uiso H133 0.00930 0.17899 0.96364 0.0362 1.0000 Uiso H141 0.25059 0.53670 0.9655 0.0300 1.0000 Uiso H142 0.25990 0.45555 1.0563 0.0300 1.0000 Uiso H143 0.09983 0.44374 0.9942 0.0300 1.0000 Uiso 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 0.01260(6) 0.01235(6) 0.01519(6) 0.00311(4) 0.00299(5) 0.00402(5) Zr2 0.01239(6) 0.01225(6) 0.01620(7) 0.00341(5) 0.00367(5) 0.00466(5) Cl1 0.02097(17) 0.03270(19) 0.01811(16) 0.00200(13) -0.00076(13) 0.00735(14) Cl2 0.02636(18) 0.02890(19) 0.01684(16) 0.00619(13) 0.00142(13) 0.00501(15) Cl3 0.01633(15) 0.02564(17) 0.02859(18) 0.00695(14) 0.00926(13) 0.00901(13) Cl4 0.02174(16) 0.01374(15) 0.03120(18) 0.00525(13) 0.00563(14) 0.00653(13) N1 0.0138(5) 0.0158(5) 0.0194(6) 0.0037(4) 0.0046(4) 0.0073(4) N2 0.0171(5) 0.0125(5) 0.0179(5) 0.0041(4) 0.0051(4) 0.0076(4) N3 0.0193(6) 0.0214(6) 0.0270(6) 0.0066(5) 0.0055(5) 0.0046(5) N4 0.0257(6) 0.0153(5) 0.0201(6) 0.0021(4) -0.0003(5) 0.0079(5) N5 0.0192(6) 0.0268(6) 0.0190(6) 0.0077(5) 0.0069(5) 0.0099(5) C1 0.0181(6) 0.0169(6) 0.0243(7) 0.0048(5) 0.0067(5) 0.0099(5) C2 0.0274(8) 0.0230(7) 0.0303(8) 0.0002(6) 0.0096(6) 0.0133(6) C3 0.0269(8) 0.0303(8) 0.0297(8) 0.0109(6) 0.0065(6) 0.0192(6) C4 0.0196(7) 0.0237(7) 0.0392(9) 0.0084(6) 0.0128(6) 0.0113(6) C5 0.0176(6) 0.0154(6) 0.0257(7) 0.0048(5) 0.0061(5) 0.0090(5) C6 0.0218(7) 0.0224(8) 0.044(1) 0.0091(7) -0.0002(7) 0.0122(6) C7 0.0516(11) 0.0274(8) 0.0359(9) 0.0077(7) 0.0243(8) 0.0244(8) C8 0.0229(7) 0.0151(6) 0.0363(8) 0.0067(6) 0.0072(6) 0.0080(6) C9 0.0271(8) 0.0346(9) 0.0331(9) 0.0108(7) 0.0146(7) 0.0021(7) C10 0.0328(9) 0.0185(8) 0.0639(12) 0.0097(7) 0.0234(9) 0.0040(7) C11 0.0320(8) 0.0254(8) 0.0189(7) 0.0001(6) 0.0038(6) 0.0063(6) C12 0.0234(8) 0.0360(9) 0.0278(8) 0.0029(6) -0.0017(6) 0.0113(7) C13 0.0341(8) 0.0297(8) 0.0259(8) 0.0136(6) 0.0075(7) 0.0114(7) C14 0.0280(8) 0.0299(8) 0.0168(7) 0.0037(6) 0.0051(6) 0.0107(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zr1 . Zr2 . 3.10010(17) yes Zr1 . Cl1 . 2.4981(4) yes Zr1 . Cl2 . 2.4934(4) yes Zr1 . N1 . 2.0111(11) yes Zr1 . N2 . 2.0210(11) yes Zr1 . N3 . 2.4894(12) yes Zr2 . Cl3 . 2.5166(3) yes Zr2 . Cl4 . 2.5382(3) yes Zr2 . N1 . 2.0877(11) yes Zr2 . N2 . 2.0735(11) yes Zr2 . N4 . 2.3971(12) yes Zr2 . N5 . 2.3809(12) yes N1 . C1 . 1.4871(16) yes N2 . C5 . 1.4908(16) yes N3 . C9 . 1.4839(19) yes N3 . C10 . 1.481(2) yes N4 . C11 . 1.4787(19) yes N4 . C12 . 1.4810(19) yes N5 . C13 . 1.4858(18) yes N5 . C14 . 1.4801(18) yes C1 . C2 . 1.5306(19) yes C1 . C3 . 1.528(2) yes C1 . C4 . 1.5320(19) yes C5 . C6 . 1.523(2) yes C5 . C7 . 1.525(2) yes C5 . C8 . 1.5356(19) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Zr2 . Zr1 . Cl1 . 102.602(9) yes Zr2 . Zr1 . Cl2 . 100.666(9) yes Cl1 . Zr1 . Cl2 . 156.107(13) yes Zr2 . Zr1 . N1 . 41.79(3) yes Cl1 . Zr1 . N1 . 100.09(3) yes Cl2 . Zr1 . N1 . 100.83(3) yes Zr2 . Zr1 . N2 . 41.43(3) yes Cl1 . Zr1 . N2 . 97.25(3) yes Cl2 . Zr1 . N2 . 96.57(3) yes N1 . Zr1 . N2 . 83.20(4) yes Zr2 . Zr1 . N3 . 174.58(3) yes Cl1 . Zr1 . N3 . 76.78(3) yes Cl2 . Zr1 . N3 . 80.57(3) yes N1 . Zr1 . N3 . 132.84(4) yes N2 . Zr1 . N3 . 143.89(4) yes Zr1 . Zr2 . Cl3 . 135.027(9) yes Zr1 . Zr2 . Cl4 . 133.123(9) yes Cl3 . Zr2 . Cl4 . 91.816(12) yes Zr1 . Zr2 . N1 . 39.94(3) yes Cl3 . Zr2 . N1 . 170.35(3) yes Cl4 . Zr2 . N1 . 94.09(3) yes Zr1 . Zr2 . N2 . 40.16(3) yes Cl3 . Zr2 . N2 . 95.27(3) yes Cl4 . Zr2 . N2 . 168.98(3) yes N1 . Zr2 . N2 . 80.08(4) yes Zr1 . Zr2 . N4 . 95.07(3) yes Cl3 . Zr2 . N4 . 89.08(3) yes Cl4 . Zr2 . N4 . 81.79(3) yes N1 . Zr2 . N4 . 99.31(4) yes N2 . Zr2 . N4 . 89.89(4) yes Zr1 . Zr2 . N5 . 98.13(3) yes Cl3 . Zr2 . N5 . 82.20(3) yes Cl4 . Zr2 . N5 . 88.53(3) yes N1 . Zr2 . N5 . 90.33(4) yes N2 . Zr2 . N5 . 100.77(4) yes N4 . Zr2 . N5 . 166.76(4) yes Zr1 . N1 . Zr2 . 98.27(5) yes Zr1 . N1 . C1 . 118.45(8) yes Zr2 . N1 . C1 . 142.76(9) yes Zr1 . N2 . Zr2 . 98.42(5) yes Zr1 . N2 . C5 . 119.56(8) yes Zr2 . N2 . C5 . 141.58(9) yes Zr1 . N3 . C9 . 120.56(9) yes Zr1 . N3 . C10 . 113.26(9) yes C9 . N3 . C10 . 109.14(12) yes Zr2 . N4 . C11 . 113.23(9) yes Zr2 . N4 . C12 . 117.31(9) yes C11 . N4 . C12 . 108.74(11) yes Zr2 . N5 . C13 . 116.71(9) yes Zr2 . N5 . C14 . 112.29(9) yes C13 . N5 . C14 . 109.84(11) yes N1 . C1 . C2 . 110.07(11) yes N1 . C1 . C3 . 109.63(11) yes C2 . C1 . C3 . 110.28(12) yes N1 . C1 . C4 . 109.45(11) yes C2 . C1 . C4 . 108.19(12) yes C3 . C1 . C4 . 109.20(12) yes N2 . C5 . C6 . 109.59(11) yes N2 . C5 . C7 . 110.10(11) yes C6 . C5 . C7 . 110.39(13) yes N2 . C5 . C8 . 109.69(11) yes C6 . C5 . C8 . 109.15(12) yes C7 . C5 . C8 . 107.89(12) yes #===end data_COMPOUND_15 _database_code_depnum_ccdc_archive 'CCDC 260438' # local code CLB12 # local code CLB12 _chemical_name_systematic ; [Zr2(mu-N-2,6-C6H3Me2)2Cl4(NC5H5)4] ; _chemical_name_common (Zr2(mu-N-2,6-C6H3Me2)2Cl4(NC5H5)4) _publ_section_exptl_refinement ; no special requirements ; # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al 2001) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 12.2186(1) _cell_length_b 12.4098(2) _cell_length_c 12.2628(2) _cell_angle_alpha 90.0000 _cell_angle_beta 105.0415(7) _cell_angle_gamma 90.0000 _cell_volume 1795.70(4) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'Zr ' -2.9673 0.5597 17.8765 1.2762 10.9480 11.9160 5.4173 0.1176 3.6572 87.6627 2.0693 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 2 _chemical_formula_sum ' C36 H38 Cl4 N6 Zr2 ' _chemical_formula_moiety ' C36 H38 Cl4 N6 Zr2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 878.99 _cell_measurement_reflns_used 4005 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _cell_measurement_temperature 150 _exptl_crystal_description ' block ' _exptl_crystal_colour ' orange ' _exptl_crystal_size_min 0.38 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_max 0.44 _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method none _exptl_crystal_F_000 888.000 _exptl_absorpt_coefficient_mu 0.914 _diffrn_measurement_device_type ; Enraf Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR97 (Altomare et al, 1999) ; _diffrn_measurement_method 'phi and omega scans' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.71 _diffrn_standards_interval_time 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_ambient_temperature 150 _diffrn_reflns_number 7336 _reflns_number_total 4100 _diffrn_reflns_av_R_equivalents 0.01 _diffrn_reflns_theta_min 2.097 _diffrn_reflns_theta_max 27.489 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.489 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _refine_ls_number_reflns 3714 _refine_ls_number_parameters 218 _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 3714 _refine_diff_density_min -0.63 _refine_diff_density_max 0.99 _refine_ls_wR_factor_ref 0.0253 _refine_ls_goodness_of_fit_ref 0.8226 _refine_ls_R_factor_all 0.0298 _refine_ls_wR_factor_all 0.0276 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_gt 0.0253 _refine_ls_shift/su_max 0.010523 _refine_ls_extinction_coef 122.1(157) _refine_ls_structure_factor_coef F _refine_ls_hydrogen_treatment 'riding model' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_hydrogens geometric _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_abs_structure_flack none _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method = Prince modified Chebychev polynomial, (Watkin, 1994) W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 1.28 0.298 0.962 0.587E-01 0.191 ; _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' ## -------------------REFERENCES ----------------------## _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. and Spagna, R. (1999) SIR97: a new tool for crystal structure determination and refinement.J. App. Cryst. 32, 115-119 COLLECT Software, Nonius BV 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_attached_hydrogens Zr1 Zr -0.11769(1) -0.01429(1) 0.02817(1) 0.0123 1.0000 Uani . N1 N -0.00480(9) -0.10614(9) -0.02493(9) 0.0140 1.0000 Uani . N2 N -0.2186(1) -0.1896(1) 0.0284(1) 0.0174 1.0000 Uani . N3 N -0.2796(1) 0.0787(1) 0.0749(1) 0.0196 1.0000 Uani . Cl1 Cl -0.07376(3) -0.04338(3) 0.23482(3) 0.0201 1.0000 Uani . Cl2 Cl -0.25518(3) 0.01367(3) -0.15776(3) 0.0198 1.0000 Uani . C1 C 0.0172(1) -0.2121(1) -0.05703(11) 0.0146 1.0000 Uani . C2 C 0.06556(11) -0.28842(11) 0.02811(12) 0.0175 1.0000 Uani . C3 C 0.09488(13) -0.39030(12) -0.00254(14) 0.0255 1.0000 Uani . C4 C 0.07642(15) -0.41884(13) -0.11552(16) 0.0336 1.0000 Uani . C5 C 0.02331(14) -0.34674(13) -0.19802(14) 0.0281 1.0000 Uani . C6 C -0.00925(11) -0.24422(11) -0.17178(12) 0.0181 1.0000 Uani . C7 C 0.08413(13) -0.26159(12) 0.15080(12) 0.0225 1.0000 Uani . C8 C -0.07840(12) -0.17661(12) -0.26707(12) 0.0215 1.0000 Uani . C9 C -0.23599(11) -0.25015(12) -0.06600(12) 0.0190 1.0000 Uani . C10 C -0.28081(13) -0.35354(12) -0.07419(13) 0.0242 1.0000 Uani . C11 C -0.31173(14) -0.39610(13) 0.01746(15) 0.0288 1.0000 Uani . C12 C -0.29581(14) -0.33484(13) 0.11496(14) 0.0269 1.0000 Uani . C13 C -0.24799(12) -0.23346(12) 0.11738(12) 0.0214 1.0000 Uani . C14 C -0.36057(14) 0.02998(13) 0.11158(16) 0.0299 1.0000 Uani . C15 C -0.45402(14) 0.08395(14) 0.12947(16) 0.0322 1.0000 Uani . C16 C -0.46349(13) 0.19349(13) 0.11017(13) 0.0248 1.0000 Uani . C17 C -0.38048(14) 0.24481(13) 0.07249(14) 0.0277 1.0000 Uani . C18 C -0.29111(13) 0.18511(13) 0.05529(14) 0.0266 1.0000 Uani . H31 H 0.12946 -0.44371 0.05760 0.0317 1.0000 Uiso . H41 H 0.10167 -0.49073 -0.13669(16) 0.0407 1.0000 Uiso . H51 H 0.00734 -0.36869 -0.27909 0.0350 1.0000 Uiso . H71 H 0.11870 -0.32494 0.19760 0.0270 1.0000 Uiso . H72 H 0.00987 -0.24369 0.16647 0.0270 1.0000 Uiso . H73 H 0.13622 -0.19829 0.17014 0.0270 1.0000 Uiso . H81 H -0.09576 -0.10560 -0.23680 0.0260 1.0000 Uiso . H82 H -0.15081 -0.21484 -0.30309 0.0260 1.0000 Uiso . H83 H -0.03462 -0.16457 -0.32449 0.0260 1.0000 Uiso . H91 H -0.21592 -0.21881 -0.13342 0.0240 1.0000 Uiso . H101 H -0.29015 -0.39651 -0.14500 0.0297 1.0000 Uiso . H111 H -0.34562 -0.46982 0.01332 0.0344 1.0000 Uiso . H121 H -0.31810 -0.36365 0.18227 0.0337 1.0000 Uiso . H131 H -0.23499 -0.19025 0.18844 0.0270 1.0000 Uiso . H141 H -0.35401 -0.04942 0.12575(16) 0.0381 1.0000 Uiso . H151 H -0.51355 0.04420 0.15591(16) 0.0423 1.0000 Uiso . H161 H -0.52892 0.23481 0.12389 0.0309 1.0000 Uiso . H171 H -0.38501 0.32414 0.05769 0.0358 1.0000 Uiso . H181 H -0.23194 0.22300 0.02657 0.0346 1.0000 Uiso . 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 0.01106(8) 0.01387(8) 0.01302(8) 0.00061(4) 0.00479(5) 0.00164(4) N1 0.0154(5) 0.0128(5) 0.0144(5) -0.0006(4) 0.0048(4) 0.0019(4) N2 0.0154(5) 0.0182(5) 0.0187(5) 0.0012(4) 0.0048(4) 0.0009(4) N3 0.0166(5) 0.0244(6) 0.0191(6) 0.0016(5) 0.0069(4) 0.0045(4) Cl1 0.02430(17) 0.02205(16) 0.01442(15) 0.00080(11) 0.00606(12) 0.00087(12) Cl2 0.01589(15) 0.02570(17) 0.01683(16) 0.00281(11) 0.00236(12) 0.00291(11) C1 0.0114(5) 0.0135(6) 0.0199(6) -0.0018(5) 0.0057(5) -0.0007(4) C2 0.0144(6) 0.0158(6) 0.0229(6) 0.0008(5) 0.0059(5) -0.0008(5) C3 0.0255(7) 0.0166(7) 0.0337(8) -0.0000(6) 0.0062(6) 0.0036(5) C4 0.0406(9) 0.0191(7) 0.0401(9) -0.0091(7) 0.0084(7) 0.0082(6) C5 0.0310(8) 0.0249(8) 0.0283(8) -0.0110(6) 0.0073(6) 0.0010(6) C6 0.0157(6) 0.0185(6) 0.0212(6) -0.0043(5) 0.0066(5) -0.0013(5) C7 0.0260(7) 0.0196(7) 0.0214(7) 0.0047(5) 0.0054(5) 0.0050(5) C8 0.0211(7) 0.0271(7) 0.0162(6) -0.0036(5) 0.0043(5) -0.0012(5) C9 0.0137(6) 0.0230(7) 0.0206(6) -0.0003(5) 0.0048(5) 0.0016(5) C10 0.0217(7) 0.0211(7) 0.0279(7) -0.0029(6) 0.0030(6) 0.0028(5) C11 0.0294(8) 0.0174(7) 0.0371(9) 0.0038(6) 0.0040(6) -0.0010(6) C12 0.0282(8) 0.0245(7) 0.0281(8) 0.0093(6) 0.0074(6) -0.0009(6) C13 0.0227(7) 0.0224(7) 0.0192(6) 0.0037(5) 0.0059(5) 0.0011(5) C14 0.0269(8) 0.0219(7) 0.047(1) 0.0090(7) 0.0205(7) 0.0055(6) C15 0.0247(7) 0.0314(8) 0.048(1) 0.0094(7) 0.0229(7) 0.0049(6) C16 0.0202(7) 0.0319(8) 0.0243(7) 0.0027(6) 0.0095(6) 0.0109(6) C17 0.0275(8) 0.0222(7) 0.0363(8) 0.0047(6) 0.0136(6) 0.0063(6) C18 0.0207(7) 0.0262(7) 0.0366(8) 0.0067(6) 0.0139(6) 0.0040(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zr1 . Zr1 2_555 3.1474(2) yes Zr1 . N1 . 2.0229(11) yes Zr1 . N1 2_555 2.1227(11) yes Zr1 . N2 . 2.5004(12) yes Zr1 . N3 . 2.4822(12) yes Zr1 . Cl1 . 2.4768(3) yes Zr1 . Cl2 . 2.4805(3) yes N1 . C1 . 1.4184(16) yes N2 . C9 . 1.3502(18) yes N2 . C13 . 1.3489(18) yes N3 . C14 . 1.333(2) yes N3 . C18 . 1.343(2) yes C1 . C2 . 1.4195(19) yes C1 . C6 . 1.4167(19) yes C2 . C3 . 1.392(2) yes C2 . C7 . 1.500(2) yes C3 . C4 . 1.391(2) yes C4 . C5 . 1.380(2) yes C5 . C6 . 1.395(2) yes C6 . C8 . 1.507(2) yes C9 . C10 . 1.388(2) yes C10 . C11 . 1.380(2) yes C11 . C12 . 1.387(2) yes C12 . C13 . 1.384(2) yes C14 . C15 . 1.389(2) yes C15 . C16 . 1.379(2) yes C16 . C17 . 1.375(2) yes C17 . C18 . 1.380(2) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Zr1 2_555 Zr1 . N1 . 41.80(3) yes Zr1 2_555 Zr1 . N1 2_555 39.44(3) yes N1 . Zr1 . N1 2_555 81.24(5) yes Zr1 2_555 Zr1 . N2 . 125.24(3) yes N1 . Zr1 . N2 . 83.55(4) yes N1 2_555 Zr1 . N2 . 164.28(4) yes Zr1 2_555 Zr1 . N3 . 145.76(3) yes N1 . Zr1 . N3 . 170.78(4) yes N1 2_555 Zr1 . N3 . 106.56(4) yes N2 . Zr1 . N3 . 88.94(4) yes Zr1 2_555 Zr1 . Cl1 . 105.86(1) yes N1 . Zr1 . Cl1 . 105.21(3) yes N1 2_555 Zr1 . Cl1 . 98.92(3) yes N2 . Zr1 . Cl1 . 81.25(3) yes N3 . Zr1 . Cl1 . 78.80(3) yes Zr1 2_555 Zr1 . Cl2 . 102.82(1) yes N1 . Zr1 . Cl2 . 97.97(3) yes N1 2_555 Zr1 . Cl2 . 101.36(3) yes N2 . Zr1 . Cl2 . 84.63(3) yes N3 . Zr1 . Cl2 . 75.93(3) yes Cl1 . Zr1 . Cl2 . 151.177(12) yes Zr1 . N1 . Zr1 2_555 98.76(5) yes Zr1 . N1 . C1 . 143.70(9) yes Zr1 2_555 N1 . C1 . 117.54(8) yes Zr1 . N2 . C9 . 116.82(9) yes Zr1 . N2 . C13 . 126.0(1) yes C9 . N2 . C13 . 116.94(12) yes Zr1 . N3 . C14 . 124.9(1) yes Zr1 . N3 . C18 . 117.9(1) yes C14 . N3 . C18 . 116.99(13) yes N1 . C1 . C2 . 119.14(11) yes N1 . C1 . C6 . 121.70(12) yes C2 . C1 . C6 . 119.16(12) yes C1 . C2 . C3 . 119.62(13) yes C1 . C2 . C7 . 121.04(12) yes C3 . C2 . C7 . 119.34(13) yes C2 . C3 . C4 . 120.91(14) yes C3 . C4 . C5 . 119.28(14) yes C4 . C5 . C6 . 122.01(15) yes C1 . C6 . C5 . 118.69(13) yes C1 . C6 . C8 . 123.45(12) yes C5 . C6 . C8 . 117.71(13) yes N2 . C9 . C10 . 123.22(14) yes C9 . C10 . C11 . 118.74(14) yes C10 . C11 . C12 . 119.03(14) yes C11 . C12 . C13 . 118.72(14) yes N2 . C13 . C12 . 123.31(14) yes N3 . C14 . C15 . 123.15(15) yes C14 . C15 . C16 . 118.93(15) yes C15 . C16 . C17 . 118.53(14) yes C16 . C17 . C18 . 118.99(15) yes N3 . C18 . C17 . 123.41(14) yes #===end