# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1648 data_global _audit_creation_date 00-03-22 _audit_creation_method CRYSTALS _publ_contact_letter ; These are the CIF format data (2 compounds) for the paper "A new and versatile diamide-donor ligand set in early transition metal chemistry" M. E. G. Skinner, D. A. Cowhig and P. Mountford* ; _publ_contact_author ; Dr P. Mountford Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK ; _publ_contact_author_phone '01865 272679' _contact_author_fax '01865 272690' _publ_contact_author_email Philip.Mountford@chem.ox.ac.uk data_COMPOUND4 # Local code MEGS7 _publ_section_exptl_refinement ; The molecules lie across crystallographic mirror planes. There is static disorder associated with the methylene carbons [C(8), C(81), C(10)] bonded to the central amino [N(3)] nitrogen. This was satisfactorily modelled ; _chemical_name_systematic ; [Ti(N-2,6-C6H3Pri2)(N2NN')] ; _cell_length_a 9.8632(4) _cell_angle_alpha 90 _cell_length_b 18.413(1) _cell_angle_beta 90 _cell_length_c 17.507(1) _cell_angle_gamma 90 _cell_volume 3179.4(8) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c m ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x,y+1/2,z' 'x,-y+1/2,-z' 'x,-y+1/2,z+1/2' '-x,y+1/2,-z+1/2' '-x,-y,z+1/2' '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' 'Si ' 0.0720 0.0710 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 'International_Tables_Vol_IV_Table_2.2B' 'Ti ' 0.2480 0.4460 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C28 H49 N5 Si2 Ti1 ' _chemical_formula_moiety ' C28 H49 N5 Si2 Ti1 ' _chemical_compound_source ; [Ti(NBu-t)(N2NN')] + H2N-2,6-C6H3Pri2 in C6D6 ; _chemical_formula_weight 559.8 _cell_measurement_reflns_used 16814 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 170 _cell_formula_units_Z 4 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_min 0.30 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_max 0.45 _exptl_crystal_density_method none _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.17 _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.36 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.879 _exptl_absorpt_correction_T_max 0.895 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-nonius DIP2000 ' _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_ambient_temperature 170 _diffrn_reflns_number 16814 _reflns_number_total 3688 _diffrn_reflns_av_R_equivalents 0.035 _reflns_number_observed 3240 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 26.42 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min 0 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _reflns_observed_criterion >3.00\s(I) _atom_sites_solution_primary 'direct methods' _atom_sites_solution_hydrogens geometric _refine_ls_matrix_type full _refine_ls_weighting_scheme 'Chebychev polynomial' _refine_ls_hydrogen_treatment riding _refine_ls_number_restraints 0 _refine_ls_abs_structure_flack none _refine_diff_density_min 0.46 _refine_diff_density_max -0.37 _refine_ls_number_reflns 3240 _refine_ls_number_parameters 198 _refine_ls_R_factor_obs 0.0574 _refine_ls_wR_factor_obs 0.0434 _refine_ls_goodness_of_fit_obs 1.1174 _refine_ls_shift/esd_max 0.0022 _refine_ls_structure_factor_coef F _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method \wA _refine_ls_extinction_coef none _refine_ls_extinction_method none _computing_data_collection 'DIP2000 software Xpress (MAC Science, 1989)' _computing_data_reduction ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SIR92 (Altomare, et al, 1994)' _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin et al, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin et al, 1996) ; _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1994)' 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_thermal_displace_type Ti1 0.09519(3) 0.00906(2) 0.7500 0.0198 1.0000 Uani N1 0.2127(2) -0.06357(9) 0.7500 0.0235 1.0000 Uani N2 0.1232(1) 0.06711(7) 0.84468(7) 0.0332 1.0000 Uani N3 -0.0999(2) 0.07658(9) 0.7500 0.0301 1.0000 Uani N4 -0.0809(2) -0.06669(9) 0.7500 0.0324 1.0000 Uani Si1 0.26278(4) 0.08050(2) 0.90295(2) 0.0329 1.0000 Uani C1 0.2732(2) -0.1307(1) 0.7500 0.0261 1.0000 Uani C2 0.3037(2) -0.16725(7) 0.8197(1) 0.0337 1.0000 Uani C3 0.3658(2) -0.23559(8) 0.8177(1) 0.0437 1.0000 Uani C4 0.3972(2) -0.2693(1) 0.750000(7) 0.0460 1.0000 Uani C5 0.2616(2) -0.1358(1) 0.8956(1) 0.0527 1.0000 Uani C6 0.1304(3) -0.1740(2) 0.9238(1) 0.0858 1.0000 Uani C7 0.3708(4) -0.1402(1) 0.9564(2) 0.1057 1.0000 Uani C8 -0.0627(3) 0.1427(2) 0.79537(1) 0.0485 0.5000 Uani C81 -0.1251(3) 0.0911(2) 0.8300(2) 0.0433 0.5000 Uani C9 0.0112(2) 0.1165(1) 0.8664(1) 0.0573 1.0000 Uani C10 -0.2148(3) 0.0385(2) 0.7146(2) 0.0377 0.5000 Uani C11 -0.2072(3) -0.0404(1) 0.7500 0.0701 1.0000 Uani C12 -0.3221(3) -0.0841(2) 0.750000(7) 0.0724 1.0000 Uani C13 -0.3065(3) -0.1564(2) 0.750000(7) 0.0704 1.0000 Uani C14 -0.1789(3) -0.1845(2) 0.750000(7) 0.0823 1.0000 Uani C15 -0.0688(3) -0.1384(1) 0.750000(7) 0.0513 1.0000 Uani C16 0.2294(2) 0.0450(1) 1.0016(1) 0.0586 1.0000 Uani C17 0.4202(2) 0.0389(1) 0.8629(1) 0.0482 1.0000 Uani C18 0.3021(3) 0.1795(1) 0.9132(2) 0.0636 1.0000 Uani H31 0.3866(2) -0.25958(8) 0.8650(1) 0.0520 1.0000 Uiso H41 0.4412(2) -0.3159(1) 0.750000(7) 0.0471 1.0000 Uiso H51 0.2450(2) -0.0852(1) 0.8858(1) 0.0622 1.0000 Uiso H61 0.1038(3) -0.1534(2) 0.9719(1) 0.1033 1.0000 Uiso H62 0.1470(3) -0.2251(2) 0.9301(1) 0.1033 1.0000 Uiso H63 0.0592(3) -0.1670(2) 0.8871(1) 0.1033 1.0000 Uiso H71 0.3389(4) -0.1193(1) 1.0033(2) 0.1181 1.0000 Uiso H72 0.3944(4) -0.1902(1) 0.9647(2) 0.1181 1.0000 Uiso H73 0.4492(4) -0.1140(1) 0.9390(2) 0.1181 1.0000 Uiso H81 -0.1429(3) 0.1693(2) 0.80876(1) 0.0623 0.5000 Uiso H82 -0.0032(3) 0.1733(2) 0.75000(1) 0.0623 0.5000 Uiso H811 -0.1556(3) 0.0473(2) 0.8544(2) 0.0609 0.5000 Uiso H812 -0.1931(3) 0.1280(2) 0.8353(2) 0.0609 0.5000 Uiso H91 0.0469(2) 0.1570(1) 0.8945(1) 0.0732 1.0000 Uiso H92 -0.0522(2) 0.0905(1) 0.8978(1) 0.0732 1.0000 Uiso H101 -0.2991(3) 0.0618(2) 0.7269(2) 0.0490 0.5000 Uiso H102 -0.2040(3) 0.0367(2) 0.6602(2) 0.0490 0.5000 Uiso H121 -0.4103(3) -0.0621(2) 0.750000(7) 0.0751 1.0000 Uiso H131 -0.3840(3) -0.1879(2) 0.750000(7) 0.0768 1.0000 Uiso H141 -0.1654(3) -0.2361(2) 0.750000(7) 0.0835 1.0000 Uiso H151 0.0208(3) -0.1588(1) 0.750000(7) 0.0622 1.0000 Uiso H161 0.3075(2) 0.0528(1) 1.0333(1) 0.0736 1.0000 Uiso H162 0.1531(2) 0.0703(1) 1.0229(1) 0.0736 1.0000 Uiso H163 0.2098(2) -0.0060(1) 0.9991(1) 0.0736 1.0000 Uiso H171 0.4948(2) 0.0475(1) 0.8970(1) 0.0599 1.0000 Uiso H172 0.4073(2) -0.0125(1) 0.8569(1) 0.0599 1.0000 Uiso H173 0.4393(2) 0.0603(1) 0.8141(1) 0.0599 1.0000 Uiso H181 0.3797(3) 0.1856(1) 0.9457(2) 0.0793 1.0000 Uiso H182 0.2254(3) 0.2037(1) 0.9354(2) 0.0793 1.0000 Uiso H183 0.3208(3) 0.2000(1) 0.8639(2) 0.0793 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 Ti1 0.0167(2) 0.0202(2) 0.0224(2) 0.0000 0.0000 0.0023(1) N1 0.0202(7) 0.0241(8) 0.0263(8) 0.0000 0.0000 0.0032(6) N2 0.0291(6) 0.0363(6) 0.0342(7) -0.0121(5) -0.0044(5) 0.0063(5) N3 0.0218(8) 0.0255(8) 0.043(1) 0.0000 0.0000 0.0030(6) N4 0.0209(8) 0.0288(8) 0.048(1) 0.0000 0.0000 -0.0006(6) Si1 0.0349(2) 0.0339(2) 0.0299(2) -0.0031(2) -0.0060(2) -0.0012(2) C1 0.0168(8) 0.0222(9) 0.039(1) 0.0000 0.0000 -0.0015(7) C2 0.0300(7) 0.0235(7) 0.0476(9) 0.0038(6) -0.0104(6) -0.0014(5) C3 0.0327(8) 0.0252(7) 0.073(1) 0.0090(8) -0.0166(8) -0.0004(5) C4 0.025(1) 0.0202(9) 0.092(2) 0.0000 0.0000 0.0012(8) C5 0.090(2) 0.0335(8) 0.0345(9) 0.0073(7) -0.0170(9) 0.0067(8) C6 0.133(3) 0.081(2) 0.043(1) 0.007(1) 0.031(1) -0.003(2) C7 0.183(4) 0.052(1) 0.082(2) -0.003(1) -0.087(2) 0.014(2) C8 0.031(2) 0.032(2) 0.083(3) -0.023(2) -0.011(2) 0.011(1) C81 0.033(2) 0.049(2) 0.049(2) -0.009(2) 0.008(1) 0.016(1) C9 0.043(1) 0.064(1) 0.065(1) -0.039(1) -0.0089(9) 0.0176(9) C10 0.024(1) 0.042(2) 0.047(2) 0.007(1) -0.006(1) 0.005(1) C11 0.024(1) 0.032(1) 0.154(4) 0.0000 0.0000 -0.0008(9) C12 0.023(1) 0.048(2) 0.146(4) 0.0000 0.0000 -0.006(1) C13 0.034(1) 0.046(1) 0.132(3) 0.0000 0.0000 -0.015(1) C14 0.039(1) 0.033(1) 0.175(4) 0.0000 0.0000 -0.004(1) C15 0.032(1) 0.030(1) 0.092(2) 0.0000 0.0000 -0.0004(9) C16 0.068(1) 0.072(1) 0.0359(9) 0.0078(9) -0.0013(9) 0.006(1) C17 0.0298(8) 0.061(1) 0.054(1) -0.0088(8) -0.0062(7) -0.0023(7) C18 0.074(1) 0.041(1) 0.076(2) -0.0082(9) -0.021(1) -0.0103(9) 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 Ti1 . N1 . 1.769(2) yes Ti1 . N2 . 1.992(1) yes Ti1 . N3 . 2.291(2) yes Ti1 . N4 . 2.227(2) yes N1 . C1 . 1.373(2) yes N2 . Si1 . 1.731(1) yes N2 . C9 . 1.481(2) yes N3 . C8 . 1.499(3) yes N3 . C81 . 1.448(4) yes N3 . C10 . 1.469(3) yes N4 . C11 . 1.337(3) yes N4 . C15 . 1.325(3) yes Si1 . C16 . 1.876(2) yes Si1 . C17 . 1.868(2) yes Si1 . C18 . 1.872(2) yes C1 . C2 . 1.425(2) yes C2 . C3 . 1.400(2) yes C2 . C5 . 1.508(3) yes C3 . C4 . 1.374(2) yes C5 . C6 . 1.554(4) yes C5 . C7 . 1.517(3) yes C8 . C9 . 1.520(3) yes C81 . C9 . 1.559(4) yes C10 . C11 . 1.580(4) yes C11 . C12 . 1.391(4) yes C12 . C13 . 1.340(5) yes C13 . C14 . 1.361(5) yes C14 . C15 . 1.379(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 N1 . Ti1 . N2 . 108.35(4) yes N2 . Ti1 . N2 8_556 112.67(8) yes N1 . Ti1 . N3 . 163.77(7) yes N2 . Ti1 . N3 . 79.94(4) yes N1 . Ti1 . N4 . 92.13(7) yes N2 . Ti1 . N4 . 116.38(4) yes N3 . Ti1 . N4 . 71.64(6) yes Ti1 . N1 . C1 . 164.9(1) yes Ti1 . N2 . Si1 . 132.64(7) yes Ti1 . N2 . C9 . 116.1(1) yes Si1 . N2 . C9 . 110.7(1) yes Ti1 . N3 . C8 . 103.6(1) yes Ti1 . N3 . C81 . 104.1(1) yes C8 8_556 N3 . C81 . 113.9(2) yes Ti1 . N3 . C10 . 112.9(1) yes C8 8_556 N3 . C10 . 110.7(2) yes C81 . N3 . C10 . 111.3(2) yes Ti1 . N4 . C11 . 120.0(2) yes Ti1 . N4 . C15 . 123.6(2) yes C11 . N4 . C15 . 116.4(2) yes N2 . Si1 . C16 . 110.70(9) yes N2 . Si1 . C17 . 112.42(7) yes C16 . Si1 . C17 . 110.4(1) yes N2 . Si1 . C18 . 111.09(9) yes C16 . Si1 . C18 . 106.7(1) yes C17 . Si1 . C18 . 105.3(1) yes N1 . C1 . C2 . 121.13(9) yes C2 . C1 . C2 8_556 117.7(2) yes C1 . C2 . C3 . 119.7(2) yes C1 . C2 . C5 . 121.0(1) yes C3 . C2 . C5 . 119.2(1) yes C2 . C3 . C4 . 121.8(2) yes C3 . C4 . C3 8_556 119.3(2) yes C2 . C5 . C6 . 109.6(2) yes C2 . C5 . C7 . 113.7(2) yes C6 . C5 . C7 . 110.1(2) yes N3 . C8 . C9 . 107.1(2) yes N3 . C81 . C9 . 107.7(2) yes C8 . C81 . C9 . 63.8(2) yes N2 . C9 . C8 . 110.0(2) yes N2 . C9 . C81 . 110.7(2) yes C8 . C9 . C81 . 49.3(2) yes N3 . C10 . C11 . 103.7(2) yes C81 8_556 C10 . C11 . 139.1(3) yes N4 . C11 . C10 . 112.2(2) yes N4 . C11 . C12 . 123.4(2) yes C10 . C11 . C12 . 119.6(2) yes C11 . C12 . C13 . 118.8(3) yes C12 . C13 . C14 . 118.9(3) yes C13 . C14 . C15 . 119.6(3) yes N4 . C15 . C14 . 122.9(2) yes #===end data_compound7 # Local code megs13 _publ_section_exptl_refinement ; No special aspects of the structure determination and refinement ; _chemical_name_systematic ; [Zr(N2NN')Cl2] ; _cell_length_a 8.4280(1) _cell_angle_alpha 90 _cell_length_b 14.3380(4) _cell_angle_beta 93.295(2) _cell_length_c 21.5020(6) _cell_angle_gamma 90 _cell_volume 2594.0 _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' 'Si ' 0.0720 0.0710 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 '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 ' C19 H35 Cl2 N4 Si2 Zr1' _chemical_formula_moiety ' C16 H32 Cl2 N4 Si2 Zr1, 0.5 (C6 H6)' _chemical_compound_source ; [Zr(CH2SiMe3)2Cl2] + H2N2NN' ; _chemical_formula_weight 537.81 _cell_measurement_reflns_used 15612 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.50 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_max 0.55 _exptl_crystal_density_diffrn 1.38 _exptl_crystal_density_method none _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1116 _exptl_absorpt_coefficient_mu 0.73 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.669 _exptl_absorpt_correction_T_max 0.694 _diffrn_radiation_monochromator graphite _diffrn_measurement_device-type 'Enraf-nonius DIP2000' _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_standards_interval_time 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method \w _diffrn_ambient_temperature 150 _diffrn_reflns_number 15612 _reflns_number_total 5550 _diffrn_reflns_av_R_equivalents 0.03 _reflns_number_observed 4506 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 26.41 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -0.29 _refine_diff_density_max 0.28 _refine_ls_number_reflns 4506 _refine_ls_number_parameters 254 _refine_ls_R_factor_obs 0.0278 _refine_ls_wR_factor_obs 0.0269 _refine_ls_goodness_of_fit_obs 1.099 _refine_ls_shift/esd_max 0.006 _refine_ls_structure_factor_coef F _refine_ls_extinction_coef 65.5(98) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eqn 22' _atom_sites_solution_primary 'Patterson' _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment 'riding model' _refine_ls_matrix_type full _refine_ls_weighting_scheme 'Chebychev polynomial' _refine_ls_number_restraints 0 _refine_ls_abs_structure_flack none _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin et al, 1996) ; _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1994)' _computing_publication_material ; CRYSTALS Issue 10 (Watkin et al, 1996) ; _computing_data_collection 'DIP2000 software Xpress (MAC Science, 1989)' _computing_data_reduction ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DIP2000 software 'DENZO' (Otwinowski & Minor, 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_thermal_displace_type Zr1 0.10885(2) 0.24967(1) 0.232697(7) 0.0273 1.0000 Uani Cl1 -0.06615(5) 0.38448(3) 0.25086(2) 0.0376 1.0000 Uani Cl2 -0.13478(5) 0.16449(4) 0.19134(2) 0.0449 1.0000 Uani N1 0.1441(2) 0.1478(1) 0.30032(7) 0.0351 1.0000 Uani N2 0.1869(2) 0.2626(1) 0.14284(7) 0.0366 1.0000 Uani N3 0.2779(2) 0.3502(1) 0.30031(6) 0.0288 1.0000 Uani N4 0.3862(2) 0.2071(1) 0.23522(7) 0.0330 1.0000 Uani C1 0.2823(2) 0.0847(1) 0.2987(1) 0.0442 1.0000 Uani C2 0.4265(2) 0.1429(1) 0.2878(1) 0.0392 1.0000 Uani C3 0.3346(2) 0.2191(2) 0.12341(9) 0.0467 1.0000 Uani C4 0.4049(2) 0.1586(2) 0.1751(1) 0.0444 1.0000 Uani C5 0.4863(2) 0.2921(1) 0.23926(9) 0.0358 1.0000 Uani C6 0.4346(2) 0.3519(1) 0.29134(8) 0.0312 1.0000 Uani C7 0.5400(2) 0.4058(1) 0.3278(1) 0.0417 1.0000 Uani C8 0.4850(2) 0.4564(1) 0.3766(1) 0.0446 1.0000 Uani C9 0.3260(2) 0.4516(1) 0.38802(9) 0.0396 1.0000 Uani C10 0.2267(2) 0.3992(1) 0.34868(8) 0.0336 1.0000 Uani C11 0.1445(3) 0.1455(2) 0.4371(1) 0.0616 1.0000 Uani C12 -0.0451(3) 0.0027(2) 0.3596(1) 0.0700 1.0000 Uani C13 -0.1489(2) 0.2056(2) 0.3606(1) 0.0508 1.0000 Uani C14 0.2036(4) 0.3759(2) 0.0285(1) 0.0718 1.0000 Uani C15 -0.0985(3) 0.3754(2) 0.0938(1) 0.0676 1.0000 Uani C16 0.0075(3) 0.2001(2) 0.0272(1) 0.0587 1.0000 Uani Si1 0.02583(6) 0.12573(4) 0.36202(2) 0.0375 1.0000 Uani Si2 0.07471(7) 0.30224(4) 0.07639(2) 0.0416 1.0000 Uani C101 0.5021(4) 0.0941(2) -0.0060(2) 0.0794 1.0000 Uani C102 0.5907(3) 0.0520(3) 0.0411(1) 0.0777 1.0000 Uani C103 0.5873(3) -0.0427(3) 0.0464(1) 0.0766 1.0000 Uani H11 0.2964(2) 0.0521(1) 0.3377(1) 0.0534 1.0000 Uiso H12 0.2657(2) 0.0404(1) 0.2655(1) 0.0534 1.0000 Uiso H21 0.4551(2) 0.1786(1) 0.3246(1) 0.0476 1.0000 Uiso H22 0.5140(2) 0.1037(1) 0.2781(1) 0.0476 1.0000 Uiso H31 0.4095(2) 0.2668(2) 0.11399(9) 0.0567 1.0000 Uiso H32 0.3111(2) 0.1817(2) 0.08702(9) 0.0567 1.0000 Uiso H41 0.5156(2) 0.1478(2) 0.1695(1) 0.0541 1.0000 Uiso H42 0.3498(2) 0.1000(2) 0.1751(1) 0.0541 1.0000 Uiso H51 0.5957(2) 0.2748(1) 0.24711(9) 0.0449 1.0000 Uiso H52 0.4744(2) 0.3260(1) 0.20079(9) 0.0449 1.0000 Uiso H71 0.6504(2) 0.4076(1) 0.3190(1) 0.0517 1.0000 Uiso H81 0.5561(2) 0.4946(1) 0.4021(1) 0.0551 1.0000 Uiso H91 0.2851(2) 0.4840(1) 0.42273(9) 0.0506 1.0000 Uiso H101 0.1154(2) 0.3975(1) 0.35594(8) 0.0436 1.0000 Uiso H111 0.0797(3) 0.1334(2) 0.4715(1) 0.0769 1.0000 Uiso H112 0.1811(3) 0.2089(2) 0.4390(1) 0.0769 1.0000 Uiso H113 0.2342(3) 0.1041(2) 0.4392(1) 0.0769 1.0000 Uiso H121 -0.1102(3) -0.0086(2) 0.3940(1) 0.0880 1.0000 Uiso H122 0.0447(3) -0.0386(2) 0.3623(1) 0.0880 1.0000 Uiso H123 -0.1061(3) -0.0082(2) 0.3212(1) 0.0880 1.0000 Uiso H131 -0.2120(2) 0.1919(2) 0.3952(1) 0.0635 1.0000 Uiso H132 -0.1123(2) 0.2689(2) 0.3635(1) 0.0635 1.0000 Uiso H133 -0.2119(2) 0.1972(2) 0.3224(1) 0.0635 1.0000 Uiso H141 0.1437(4) 0.3980(2) -0.0079(1) 0.0873 1.0000 Uiso H142 0.2421(4) 0.4281(2) 0.0529(1) 0.0873 1.0000 Uiso H143 0.2919(4) 0.3395(2) 0.0161(1) 0.0873 1.0000 Uiso H151 -0.1538(3) 0.3945(2) 0.0556(1) 0.0803 1.0000 Uiso H152 -0.0626(3) 0.4296(2) 0.1168(1) 0.0803 1.0000 Uiso H153 -0.1689(3) 0.3399(2) 0.1182(1) 0.0803 1.0000 Uiso H161 -0.0537(3) 0.2217(2) -0.0089(1) 0.0756 1.0000 Uiso H162 -0.0568(3) 0.1597(2) 0.0510(1) 0.0756 1.0000 Uiso H163 0.0986(3) 0.1664(2) 0.0145(1) 0.0756 1.0000 Uiso H1011 0.5034(4) 0.1608(2) -0.0101(2) 0.0996 1.0000 Uiso H1021 0.6550(3) 0.0887(3) 0.0702(1) 0.0928 1.0000 Uiso H1031 0.6493(3) -0.0728(3) 0.0795(1) 0.0920 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 0.01880(8) 0.03267(9) 0.03033(9) -0.00283(7) 0.00089(5) 0.00332(6) Cl1 0.0282(2) 0.0415(2) 0.0429(2) -0.0038(2) 0.0006(2) 0.0111(2) Cl2 0.0265(2) 0.0559(3) 0.0517(3) -0.0121(2) -0.0037(2) -0.0044(2) N1 0.0280(7) 0.0334(8) 0.0436(8) 0.0034(6) -0.0012(6) 0.0011(6) N2 0.0283(7) 0.0488(9) 0.0328(7) -0.0063(7) 0.0032(6) 0.0039(6) N3 0.0244(7) 0.0301(7) 0.0319(7) -0.0010(6) 0.0018(5) 0.0016(5) N4 0.0218(7) 0.0363(8) 0.0405(8) -0.0078(6) -0.0002(6) 0.0048(6) C1 0.037(1) 0.033(1) 0.062(1) 0.0016(9) -0.0010(9) 0.0075(8) C2 0.0270(8) 0.037(1) 0.053(1) -0.0024(8) -0.0054(8) 0.0098(7) C3 0.0311(9) 0.070(1) 0.039(1) -0.0169(9) 0.0056(8) 0.0059(9) C4 0.0261(8) 0.054(1) 0.053(1) -0.023(1) 0.0011(8) 0.0089(8) C5 0.0224(8) 0.042(1) 0.043(1) -0.0069(8) 0.0048(7) 0.0002(7) C6 0.0239(8) 0.0334(9) 0.0363(9) 0.0007(7) 0.0008(7) 0.0019(7) C7 0.0290(9) 0.044(1) 0.052(1) -0.0083(9) 0.0011(8) -0.0041(8) C8 0.040(1) 0.043(1) 0.050(1) -0.0098(9) -0.0051(8) -0.0050(8) C9 0.042(1) 0.039(1) 0.0374(9) -0.0070(8) 0.0013(8) 0.0012(8) C10 0.0296(8) 0.0366(9) 0.0348(9) -0.0018(7) 0.0034(7) 0.0015(7) C11 0.060(1) 0.075(2) 0.047(1) -0.002(1) -0.016(1) 0.006(1) C12 0.075(2) 0.052(1) 0.082(2) 0.011(1) 0.002(1) -0.025(1) C13 0.039(1) 0.073(1) 0.041(1) 0.009(1) 0.0076(8) 0.004(1) C14 0.093(2) 0.080(2) 0.043(1) 0.004(1) 0.006(1) -0.017(2) C15 0.074(2) 0.089(2) 0.039(1) 0.003(1) -0.004(1) 0.039(1) C16 0.056(1) 0.066(2) 0.052(1) -0.012(1) -0.014(1) 0.001(1) Si1 0.0352(3) 0.0394(3) 0.0373(3) 0.0050(2) -0.0038(2) -0.0055(2) Si2 0.0433(3) 0.0516(3) 0.0296(2) -0.0042(2) 0.0006(2) 0.0055(2) C101 0.073(2) 0.060(2) 0.111(3) 0.008(2) 0.052(2) 0.008(1) C102 0.053(1) 0.124(3) 0.058(2) -0.031(2) 0.025(1) -0.025(2) C103 0.046(1) 0.127(3) 0.058(2) 0.036(2) 0.012(1) 0.016(2) 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 . 2.4760(4) yes Zr1 . Cl2 . 2.5077(5) yes Zr1 . N1 . 2.070(2) yes Zr1 . N2 . 2.085(2) yes Zr1 . N3 . 2.446(1) yes Zr1 . N4 . 2.414(1) yes N1 . C1 . 1.477(2) yes N1 . Si1 . 1.734(2) yes N2 . C3 . 1.474(2) yes N2 . Si2 . 1.761(2) yes N3 . C6 . 1.345(2) yes N3 . C10 . 1.347(2) yes N4 . C2 . 1.483(2) yes N4 . C4 . 1.484(2) yes N4 . C5 . 1.481(2) yes C1 . C2 . 1.504(3) yes C3 . C4 . 1.504(3) yes C5 . C6 . 1.495(2) yes C6 . C7 . 1.386(3) yes C7 . C8 . 1.378(3) yes C8 . C9 . 1.378(3) yes C9 . C10 . 1.377(3) yes C11 . Si1 . 1.871(2) yes C12 . Si1 . 1.862(2) yes C13 . Si1 . 1.864(2) yes C14 . Si2 . 1.867(3) yes C15 . Si2 . 1.853(2) yes C16 . Si2 . 1.875(2) yes C101 . C102 . 1.364(5) yes C101 . C103 2_655 1.339(5) yes C102 . C103 . 1.363(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 Cl1 . Zr1 . Cl2 . 87.31(2) yes Cl1 . Zr1 . N1 . 120.17(4) yes Cl2 . Zr1 . N1 . 89.25(4) yes Cl1 . Zr1 . N2 . 107.40(4) yes Cl2 . Zr1 . N2 . 90.58(4) yes N1 . Zr1 . N2 . 132.35(6) yes Cl1 . Zr1 . N3 . 77.19(3) yes Cl2 . Zr1 . N3 . 159.21(3) yes N1 . Zr1 . N3 . 86.73(5) yes N2 . Zr1 . N3 . 107.13(5) yes Cl1 . Zr1 . N4 . 141.14(4) yes Cl2 . Zr1 . N4 . 131.09(4) yes N1 . Zr1 . N4 . 72.93(6) yes N2 . Zr1 . N4 . 71.74(5) yes N3 . Zr1 . N4 . 66.74(5) yes Zr1 . N1 . C1 . 119.8(1) yes Zr1 . N1 . Si1 . 126.93(8) yes C1 . N1 . Si1 . 113.2(1) yes Zr1 . N2 . C3 . 122.8(1) yes Zr1 . N2 . Si2 . 126.69(8) yes C3 . N2 . Si2 . 109.2(1) yes Zr1 . N3 . C6 . 117.9(1) yes Zr1 . N3 . C10 . 124.4(1) yes C6 . N3 . C10 . 117.5(1) yes Zr1 . N4 . C2 . 110.7(1) yes Zr1 . N4 . C4 . 104.5(1) yes C2 . N4 . C4 . 110.0(2) yes Zr1 . N4 . C5 . 109.9(1) yes C2 . N4 . C5 . 111.2(1) yes C4 . N4 . C5 . 110.4(1) yes N1 . C1 . C2 . 108.0(2) yes N4 . C2 . C1 . 108.2(1) yes N2 . C3 . C4 . 109.7(2) yes N4 . C4 . C3 . 108.4(2) yes N4 . C5 . C6 . 109.0(1) yes N3 . C6 . C5 . 115.3(1) yes N3 . C6 . C7 . 122.1(2) yes C5 . C6 . C7 . 122.5(2) yes C6 . C7 . C8 . 119.4(2) yes C7 . C8 . C9 . 118.9(2) yes C8 . C9 . C10 . 118.7(2) yes N3 . C10 . C9 . 123.3(2) yes N1 . Si1 . C11 . 109.3(1) yes N1 . Si1 . C12 . 110.4(1) yes C14 . Si1 . C12 . 108.8(1) yes N1 . Si1 . C13 . 111.31(9) yes C14 . Si1 . C13 . 107.7(1) yes C15 . Si1 . C13 . 109.2(1) yes N2 . Si2 . C14 . 109.1(1) yes N2 . Si2 . C15 . 114.28(9) yes C11 . Si2 . C15 . 106.3(1) yes N2 . Si2 . C16 . 109.6(1) yes C11 . Si2 . C16 . 107.3(1) yes C12 . Si2 . C16 . 109.9(1) yes C102 . C101 . C103 2_655 120.1(3) yes C101 . C102 . C103 . 119.3(3) yes C101 2_655 C103 . C102 . 120.5(3) yes #=== end