data_global _audit_creation_date 6-04-03 _audit_creation_method CRYSTALS _publ_contact_letter ; These are the *NEW* CIF format data (2 compounds) for the paper "Group 6 Imido Complexes Supported by Diamido-Donor Ligands B. D. Ward, S. R. Dubberley, L. H. Gade and P. Mountford submitted to Inorganic Chemistry. Reference ID: IC034377S ; _publ_contact_author ; Dr P. Mountford Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK ; _publ_contact_author_phone '+44 1865 272679 _contact_author_fax '+44 1865 272690' _publ_contact_author_email Philip.Mountford@chem.ox.ac.uk _publ_requested_journal 'Inorganic Chemistry' data_compound_5 # Local code BDW5 _chemical_name_systematic ; [W{(2-C5NH4)C(Me)(CH2NSiMe3)2}(NPh)Me2] ; _publ_section_exptl_refinement ; No special details ; _cell_length_a 10.6452(2) _cell_length_b 16.4633(3) _cell_length_c 15.2794(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.659(1) _cell_angle_gamma 90.00 _cell_volume 2676.67(8) _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' 'W ' -1.4210 6.8720 29.0818 1.7203 15.4300 9.2259 14.4327 0.3217 5.1198 57.0560 9.8875 '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' _chemical_formula_sum ' C23 H40 N4 Si2 W1 ' _chemical_formula_moiety ' C23 H40 N4 Si2 W1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 612.62 _cell_measurement_temperature 150 _cell_measurement_reflns_used 6261 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _cell_formula_units_Z 4 _exptl_crystal_description 'block ' _exptl_crystal_colour 'dark red' _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.52 _exptl_crystal_density_method none _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1227.09 _exptl_absorpt_coefficient_mu 4.42 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.413 _exptl_absorpt_correction_T_max 0.643 _diffrn_ambient_temperature 150 _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_reflns_number 12044 _reflns_number_total 6111 _diffrn_reflns_av_R_equivalents 0.01 _reflns_number_gt 4338 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _refine_diff_density_min -0.60 _refine_diff_density_max 1.19 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 4338 _refine_ls_number_parameters 272 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0106 _refine_ls_goodness_of_fit_ref 1.2430 _refine_ls_shift/su_max 0.01 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 'Chebychev polynomial' _refine_ls_weighting_details ; Chebychev polynomial with 2 parameters, Carruthers & Watkin , 1979, 0.828E-01-.519 ; _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_extinction_coef 71.1(39) _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 W1 0.237863(6) 0.247246(7) 0.386340(4) 0.0172 1.0000 Uani N1 0.10629(18) 0.30981(11) 0.39420(12) 0.0216 1.0000 Uani N2 0.22724(17) 0.1635(1) 0.48039(11) 0.0207 1.0000 Uani N3 0.19528(16) 0.15889(11) 0.2965(1) 0.0201 1.0000 Uani N4 0.43910(17) 0.19381(11) 0.37012(11) 0.0222 1.0000 Uani Si1 0.11065(6) 0.16617(4) 0.56007(4) 0.0261 1.0000 Uani Si2 0.10304(5) 0.16757(4) 0.20055(4) 0.0227 1.0000 Uani C1 0.0234(2) 0.37564(12) 0.39351(13) 0.0197 1.0000 Uani C2 0.0675(2) 0.45246(14) 0.37170(16) 0.0290 1.0000 Uani C3 -0.0154(3) 0.51753(15) 0.36860(17) 0.0368 1.0000 Uani C4 -0.1399(3) 0.50687(15) 0.38618(18) 0.0356 1.0000 Uani C5 -0.1836(2) 0.43054(16) 0.40947(18) 0.0346 1.0000 Uani C6 -0.1028(2) 0.36493(15) 0.41378(15) 0.0290 1.0000 Uani C7 0.3051(2) 0.32113(13) 0.27299(13) 0.0269 1.0000 Uani C8 0.3512(2) 0.32977(14) 0.47298(14) 0.0273 1.0000 Uani C9 0.53839(19) 0.2426(2) 0.35656(12) 0.0285 1.0000 Uani C10 0.6569(2) 0.21364(17) 0.33946(16) 0.0336 1.0000 Uani C11 0.6748(2) 0.13045(19) 0.33521(18) 0.0391 1.0000 Uani C12 0.5740(2) 0.07971(17) 0.35014(15) 0.0307 1.0000 Uani C13 0.4563(2) 0.11259(13) 0.36734(14) 0.0225 1.0000 Uani C14 0.3419(2) 0.06276(14) 0.38534(14) 0.0252 1.0000 Uani C15 0.3715(2) -0.02865(14) 0.38796(17) 0.0310 1.0000 Uani C16 0.2926(2) 0.08577(13) 0.47581(15) 0.0248 1.0000 Uani C17 0.2401(2) 0.07519(12) 0.31209(15) 0.0264 1.0000 Uani C18 -0.0387(3) 0.12820(18) 0.5087(2) 0.0512 1.0000 Uani C19 0.0881(2) 0.26955(13) 0.60582(15) 0.0309 1.0000 Uani C20 0.1575(3) 0.09837(17) 0.65424(19) 0.0498 1.0000 Uani C21 0.0135(3) 0.07131(16) 0.18181(18) 0.0399 1.0000 Uani C22 -0.01582(17) 0.2509(2) 0.20680(13) 0.0302 1.0000 Uani C23 0.2017(2) 0.18346(19) 0.10303(15) 0.0383 1.0000 Uani H21 0.1582 0.46038 0.35847 0.0360 1.0000 Uiso H31 0.0163 0.57277 0.35333 0.0442 1.0000 Uiso H41 -0.1992 0.55392 0.38250 0.0433 1.0000 Uiso H51 -0.2743 0.42279 0.42274 0.0410 1.0000 Uiso H61 -0.1339 0.31020 0.43150 0.0358 1.0000 Uiso H71 0.3860 0.29812 0.25228 0.0351 1.0000 Uiso H72 0.3188 0.37871 0.29208 0.0351 1.0000 Uiso H73 0.2406 0.31964 0.22411 0.0351 1.0000 Uiso H81 0.4380 0.30757 0.48086 0.0354 1.0000 Uiso H82 0.3110 0.33390 0.53118 0.0354 1.0000 Uiso H83 0.3548 0.38488 0.44561 0.0354 1.0000 Uiso H91 0.52550 0.3027 0.35899 0.0351 1.0000 Uiso H101 0.7286 0.25165 0.33032 0.0433 1.0000 Uiso H111 0.7589 0.10737 0.32158 0.0461 1.0000 Uiso H121 0.5851 0.01941 0.34874 0.0375 1.0000 Uiso H151 0.2930 -0.05954 0.40021 0.0395 1.0000 Uiso H152 0.4362 -0.03974 0.43521 0.0395 1.0000 Uiso H153 0.4043 -0.04614 0.33025 0.0395 1.0000 Uiso H161 0.3661 0.08748 0.51811 0.0315 1.0000 Uiso H162 0.2330 0.04232 0.49377 0.0315 1.0000 Uiso H171 0.1656 0.04149 0.32722 0.0338 1.0000 Uiso H172 0.2755 0.05497 0.25623 0.0338 1.0000 Uiso H181 -0.1069 0.12886 0.5523 0.0621 1.0000 Uiso H182 -0.0261 0.07141 0.4875 0.0621 1.0000 Uiso H183 -0.0628 0.16398 0.4581 0.0621 1.0000 Uiso H191 0.0213 0.26798 0.65049 0.0391 1.0000 Uiso H192 0.1688 0.28862 0.63397 0.0391 1.0000 Uiso H193 0.0623 0.30770 0.55764 0.0391 1.0000 Uiso H201 0.0914 0.09979 0.69937 0.0624 1.0000 Uiso H202 0.2390 0.11798 0.68071 0.0624 1.0000 Uiso H203 0.1678 0.04143 0.63281 0.0624 1.0000 Uiso H211 -0.0395 0.07617 0.12696 0.0498 1.0000 Uiso H212 -0.0416 0.06100 0.23253 0.0498 1.0000 Uiso H213 0.0738 0.02518 0.17591 0.0498 1.0000 Uiso H221 -0.06626 0.2536 0.15063 0.0383 1.0000 Uiso H222 0.02826 0.3039 0.21699 0.0383 1.0000 Uiso H223 -0.07292 0.2399 0.25625 0.0383 1.0000 Uiso H231 0.1464 0.18826 0.04929 0.0490 1.0000 Uiso H232 0.2518 0.23447 0.11104 0.0490 1.0000 Uiso H233 0.2601 0.13635 0.09659 0.0490 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 W1 0.01658(4) 0.01740(4) 0.01751(4) 0.00054(6) 0.000983(19) 0.00129(6) N1 0.0221(8) 0.0223(8) 0.0206(8) 0.0010(7) 0.0023(6) -0.0004(7) N2 0.0235(8) 0.0190(7) 0.0198(8) 0.0007(7) 0.0024(6) 0.0032(7) N3 0.0200(8) 0.0198(8) 0.0203(8) 0.0018(6) -0.0034(6) 0.0015(7) N4 0.0207(8) 0.0258(8) 0.0201(8) -0.0010(6) 0.0001(6) 0.0017(7) Si1 0.0273(3) 0.0225(3) 0.0289(3) 0.0032(2) 0.0085(2) 0.0017(2) Si2 0.0199(3) 0.0275(3) 0.0206(3) -0.0017(2) -0.0020(2) 0.0025(2) C1 0.022(1) 0.0213(9) 0.0157(9) -0.0007(7) 0.0001(7) 0.0054(8) C2 0.0304(12) 0.022(1) 0.0352(12) 0.0009(9) 0.0041(9) 0.0022(9) C3 0.0456(14) 0.0251(11) 0.0401(14) 0.006(1) 0.0059(11) 0.008(1) C4 0.0372(12) 0.0307(11) 0.0390(13) -0.0014(9) 0.001(1) 0.016(1) C5 0.0253(11) 0.0388(14) 0.0400(14) -0.003(1) 0.006(1) 0.011(1) C6 0.0279(12) 0.0266(11) 0.0327(12) -0.0008(9) 0.0061(9) 0.0027(9) C7 0.029(1) 0.0295(11) 0.0225(11) 0.0066(8) 0.0088(9) -0.0038(9) C8 0.0306(11) 0.025(1) 0.026(1) -0.0091(9) -0.0018(9) -0.0038(9) C9 0.0254(9) 0.0364(14) 0.0238(8) -0.0019(12) 0.0000(7) -0.0022(12) C10 0.023(1) 0.0483(13) 0.0295(12) -0.0028(11) 0.0009(8) -0.005(1) C11 0.0226(11) 0.0601(17) 0.0348(13) -0.0015(13) 0.0032(9) 0.0107(12) C12 0.0271(11) 0.0388(12) 0.0262(11) -0.001(1) 0.0010(9) 0.008(1) C13 0.0201(11) 0.0284(11) 0.0188(9) -0.0001(8) -0.0031(7) 0.0039(9) C14 0.021(1) 0.0264(11) 0.0278(11) -0.0002(8) -0.0025(8) 0.0037(8) C15 0.0300(11) 0.025(1) 0.0384(12) -0.0023(9) -0.0033(9) 0.0077(9) C16 0.027(1) 0.0220(9) 0.026(1) 0.0048(9) 0.0038(8) 0.0054(9) C17 0.0289(11) 0.0185(9) 0.0314(11) -0.0030(8) -0.0064(9) 0.0020(9) C18 0.0275(12) 0.0395(14) 0.087(2) -0.0110(15) 0.0138(14) -0.0046(11) C19 0.0380(11) 0.0303(13) 0.0253(9) -0.0002(8) 0.0124(8) 0.0036(8) C20 0.074(2) 0.0412(14) 0.0360(14) 0.0159(11) 0.0269(14) 0.0150(14) C21 0.0412(15) 0.0369(14) 0.0404(15) -0.000(1) -0.0163(12) -0.0017(11) C22 0.0246(8) 0.0355(9) 0.0302(8) -0.0046(18) -0.0066(7) 0.0095(17) C23 0.0263(12) 0.0690(18) 0.020(1) -0.0032(11) 0.0015(9) 0.0008(12) 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 W1 . N1 . 1.7455(18) yes W1 . N2 . 1.9968(17) yes W1 . N3 . 2.0416(17) yes W1 . N4 . 2.3357(18) yes W1 . C7 . 2.250(2) yes W1 . C8 . 2.228(2) yes N1 . C1 . 1.397(3) yes N2 . Si1 . 1.7641(18) yes N2 . C16 . 1.460(3) yes N3 . Si2 . 1.7471(17) yes N3 . C17 . 1.475(3) yes N4 . C9 . 1.348(3) yes N4 . C13 . 1.350(3) yes Si1 . C18 . 1.860(3) yes Si1 . C19 . 1.858(2) yes Si1 . C20 . 1.877(3) yes Si2 . C21 . 1.867(3) yes Si2 . C22 . 1.871(3) yes Si2 . C23 . 1.866(3) yes C1 . C2 . 1.393(3) yes C1 . C6 . 1.399(3) yes C2 . C3 . 1.388(3) yes C3 . C4 . 1.371(4) yes C4 . C5 . 1.390(4) yes C5 . C6 . 1.382(3) yes C9 . C10 . 1.380(3) yes C10 . C11 . 1.385(4) yes C11 . C12 . 1.384(4) yes C12 . C13 . 1.397(3) yes C13 . C14 . 1.500(3) yes C14 . C15 . 1.538(3) yes C14 . C16 . 1.540(3) yes C14 . C17 . 1.549(3) 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 . W1 . N2 . 107.19(8) yes N1 . W1 . N3 . 107.68(8) yes N2 . W1 . N3 . 88.61(7) yes N1 . W1 . N4 . 165.89(7) yes N2 . W1 . N4 . 83.55(7) yes N3 . W1 . N4 . 81.19(7) yes N1 . W1 . C7 . 90.45(8) yes N2 . W1 . C7 . 162.36(8) yes N3 . W1 . C7 . 86.40(7) yes N4 . W1 . C7 . 78.97(7) yes N1 . W1 . C8 . 91.21(9) yes N2 . W1 . C8 . 91.97(8) yes N3 . W1 . C8 . 160.03(8) yes N4 . W1 . C8 . 79.05(8) yes C7 . W1 . C8 . 87.06(8) yes W1 . N1 . C1 . 164.76(16) yes W1 . N2 . Si1 . 122.36(9) yes W1 . N2 . C16 . 122.26(14) yes Si1 . N2 . C16 . 113.63(14) yes W1 . N3 . Si2 . 127.9(1) yes W1 . N3 . C17 . 119.53(13) yes Si2 . N3 . C17 . 112.51(13) yes W1 . N4 . C9 . 121.17(17) yes W1 . N4 . C13 . 120.13(15) yes C9 . N4 . C13 . 118.5(2) yes N2 . Si1 . C18 . 108.08(12) yes N2 . Si1 . C19 . 112.5(1) yes C18 . Si1 . C19 . 110.39(12) yes N2 . Si1 . C20 . 109.72(11) yes C18 . Si1 . C20 . 109.17(16) yes C19 . Si1 . C20 . 106.90(13) yes N3 . Si2 . C21 . 109.4(1) yes N3 . Si2 . C22 . 112.43(9) yes C21 . Si2 . C22 . 106.69(12) yes N3 . Si2 . C23 . 111.5(1) yes C21 . Si2 . C23 . 107.06(13) yes C22 . Si2 . C23 . 109.58(12) yes N1 . C1 . C2 . 119.29(18) yes N1 . C1 . C6 . 120.7(2) yes C2 . C1 . C6 . 120.0(2) yes C1 . C2 . C3 . 119.4(2) yes C2 . C3 . C4 . 120.8(2) yes C3 . C4 . C5 . 119.9(2) yes C4 . C5 . C6 . 120.4(2) yes C1 . C6 . C5 . 119.5(2) yes N4 . C9 . C10 . 123.3(3) yes C9 . C10 . C11 . 118.6(3) yes C10 . C11 . C12 . 118.7(2) yes C11 . C12 . C13 . 120.1(2) yes N4 . C13 . C12 . 120.8(2) yes N4 . C13 . C14 . 115.09(18) yes C12 . C13 . C14 . 124.1(2) yes C13 . C14 . C15 . 111.91(18) yes C13 . C14 . C16 . 109.23(18) yes C15 . C14 . C16 . 106.99(18) yes C13 . C14 . C17 . 110.49(18) yes C15 . C14 . C17 . 106.66(18) yes C16 . C14 . C17 . 111.52(17) yes N2 . C16 . C14 . 115.72(18) yes N3 . C17 . C14 . 117.14(17) yes #===end data_compound_6 # Local code BDW2 _publ_section_exptl_refinement ; The crystal was a poor diffractor. The choice of non-centrosymmetric space group was supported by an examination of the normalised structure factors (SIR92) and successful refinement. Satisfactory anisotropic refinement was achieved subject to loose vibrational restraints to most non-H atoms, planarity restraints on the phenyl and pyridyl rings and similarity restraints on the internal angles of the C(1)-C(6) ring. ; _chemical_name_systematic ; [W{(2-C5NH4)C(Me)(CH2NSiMe3)2}(NPh)Ph2] ; _cell_length_a 9.6367(5) _cell_angle_alpha 90 _cell_length_b 17.1252(11) _cell_angle_beta 108.1435(28) _cell_length_c 10.4777(5) _cell_angle_gamma 90 _cell_volume 1643.2(6) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,y+1/2,-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' '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' 'W ' -1.4210 6.8720 29.0818 1.7203 15.4300 9.2259 14.4327 0.3217 5.1198 57.0560 9.8875 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C33 H44 N4 Si2 W1 ' _chemical_formula_moiety ' C33 H44 N4 Si2 W1 ' _chemical_formula_weight 736.76 _cell_measurement_reflns_used 5881 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _cell_measurement_temperature 150 _cell_formula_units_Z 2 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.49 _exptl_crystal_density_method none _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 741.54 _exptl_absorpt_coefficient_mu 3.62 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.337 _exptl_absorpt_correction_T_max 0.696 _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' _refine_ls_extinction_method 'None' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _diffrn_ambient_temperature 150 _diffrn_reflns_number 11744 _reflns_number_total 6948 _diffrn_reflns_av_R_equivalents 0.07 _reflns_number_gt 3096 _diffrn_reflns_theta_min 2.910 _diffrn_reflns_theta_max 27.485 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _reflns_limit_h_min -12 _reflns_limit_h_max 11 _reflns_limit_k_min -21 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 13 _refine_diff_density_min -0.97 _refine_diff_density_max 0.87 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 3096 _refine_ls_number_parameters 361 _refine_ls_R_factor_gt 0.0642 _refine_ls_wR_factor_ref 0.0683 _refine_ls_goodness_of_fit_ref 0.9146 _refine_ls_shift/su_max 0.0019 _refine_ls_abs_structure_Flack '0.20(3)' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_hydrogens geometric _refine_ls_matrix_type full _refine_ls_number_restraints 382 _refine_ls_extinction_coef 'none required' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 'Chebychev polynomial' _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 0.640 -.336E-010.307 ; _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 W1 0.98361(6) 0.14544(17) 0.74610(8) 0.0339 1.0000 Uani N1 0.9172(14) 0.1750(9) 0.8783(15) 0.0361 1.0000 Uani N2 1.1395(14) 0.223(1) 0.7499(16) 0.0345 1.0000 Uani N3 0.8498(14) 0.207(1) 0.5896(15) 0.0344 1.0000 Uani N4 1.0644(9) 0.0885(9) 0.5831(12) 0.0349 1.0000 Uani Si1 1.2478(6) 0.2772(5) 0.8918(7) 0.0504 1.0000 Uani Si2 0.6719(6) 0.2371(4) 0.5767(7) 0.0479 1.0000 Uani C1 0.8586(11) 0.1927(11) 0.9819(11) 0.0384 1.0000 Uani C2 0.789(1) 0.137(1) 1.0331(11) 0.0390 1.0000 Uani C3 0.727(1) 0.159(1) 1.1334(12) 0.0392 1.0000 Uani C4 0.7352(11) 0.2318(11) 1.1783(11) 0.0391 1.0000 Uani C5 0.8042(12) 0.2881(9) 1.1282(13) 0.0393 1.0000 Uani C6 0.8668(11) 0.269(1) 1.0300(13) 0.0391 1.0000 Uani C7 1.1554(17) 0.0692(8) 0.8725(18) 0.0356 1.0000 Uani C8 1.2872(17) 0.0571(9) 0.853(2) 0.0365 1.0000 Uani C9 1.4050(19) 0.0083(8) 0.9462(18) 0.0367 1.0000 Uani C10 1.3757(18) -0.0242(8) 1.0540(18) 0.0364 1.0000 Uani C11 1.2410(17) -0.0121(8) 1.0758(18) 0.0366 1.0000 Uani C12 1.1319(18) 0.0328(8) 0.9882(17) 0.0367 1.0000 Uani C13 0.8302(16) 0.0463(9) 0.690(2) 0.0358 1.0000 Uani C14 0.7325(17) 0.0429(11) 0.543(2) 0.0365 1.0000 Uani C15 0.6283(17) -0.010(1) 0.503(2) 0.0365 1.0000 Uani C16 0.6046(17) -0.064(1) 0.591(2) 0.0364 1.0000 Uani C17 0.6891(16) -0.066(1) 0.728(2) 0.0365 1.0000 Uani C18 0.8054(16) -0.0059(9) 0.770(2) 0.0364 1.0000 Uani C19 1.083(1) 0.0117(11) 0.5800(13) 0.0352 1.0000 Uani C20 1.120(1) -0.0215(9) 0.4776(16) 0.0353 1.0000 Uani C21 1.139(1) 0.0286(12) 0.3688(14) 0.0353 1.0000 Uani C22 1.120(1) 0.104(1) 0.3738(14) 0.0352 1.0000 Uani C23 1.0831(9) 0.1369(9) 0.4794(12) 0.0352 1.0000 Uani C24 1.0672(14) 0.2201(11) 0.4937(15) 0.0353 1.0000 Uani C25 1.1003(19) 0.2733(12) 0.3873(19) 0.0356 1.0000 Uani C26 1.1753(17) 0.2460(12) 0.6297(16) 0.0351 1.0000 Uani C27 0.9043(15) 0.2372(13) 0.4822(19) 0.0349 1.0000 Uani C28 1.168(2) 0.3807(14) 0.883(2) 0.0507 1.0000 Uani C29 1.439(2) 0.2815(15) 0.888(2) 0.0506 1.0000 Uani C30 1.251(2) 0.2339(14) 1.053(2) 0.0505 1.0000 Uani C31 0.682(2) 0.3324(14) 0.656(3) 0.0483 1.0000 Uani C32 0.5583(19) 0.2408(15) 0.392(2) 0.0480 1.0000 Uani C33 0.5683(18) 0.1745(13) 0.663(2) 0.0478 1.0000 Uani H21 0.787 0.083 0.9963 0.0429 1.0000 Uiso H31 0.680 0.116 1.1693 0.0431 1.0000 Uiso H51 0.8064 0.3423 1.1643 0.0431 1.0000 Uiso H61 0.9145 0.312 0.9934 0.0430 1.0000 Uiso H81 1.2996 0.0814 0.770 0.0414 1.0000 Uiso H101 1.4506 -0.0563 1.1209 0.0414 1.0000 Uiso H111 1.2225 -0.0352 1.1566 0.0415 1.0000 Uiso H121 1.0369 0.0401 1.0064 0.0416 1.0000 Uiso H141 0.7451 0.0825 0.478 0.0413 1.0000 Uiso H151 0.5629 -0.011 0.408 0.0413 1.0000 Uiso H161 0.5257 -0.104 0.558 0.0413 1.0000 Uiso H171 0.6748 -0.105 0.793 0.0413 1.0000 Uiso H181 0.8703 -0.0060 0.865 0.0413 1.0000 Uiso H191 1.071 -0.0217 0.6540 0.0408 1.0000 Uiso H201 1.133 -0.0793 0.4743 0.0409 1.0000 Uiso H211 1.163 0.0050 0.2909 0.0408 1.0000 Uiso H221 1.133 0.138 0.3009 0.0408 1.0000 Uiso H251 1.0823 0.3283 0.4104 0.0411 1.0000 Uiso H252 1.2062 0.2665 0.3972 0.0411 1.0000 Uiso H253 1.0406 0.2620 0.2925 0.0411 1.0000 Uiso H261 1.2739 0.2253 0.6349 0.0407 1.0000 Uiso H262 1.1777 0.3044 0.6303 0.0407 1.0000 Uiso H271 0.8930 0.2951 0.4845 0.0406 1.0000 Uiso H272 0.8419 0.2166 0.3936 0.0406 1.0000 Uiso H301 1.313 0.2663 1.129 0.0610 1.0000 Uiso H302 1.292 0.1800 1.059 0.0610 1.0000 Uiso H303 1.149 0.2314 1.058 0.0610 1.0000 Uiso H311 0.582 0.3514 0.649 0.0609 1.0000 Uiso H312 0.742 0.3280 0.753 0.0609 1.0000 Uiso H313 0.730 0.3701 0.610 0.0609 1.0000 Uiso H91 1.5003 0.0011 0.9285 0.0450 1.0000 Uiso H41 0.6892 0.2429 1.2497 0.0466 1.0000 Uiso H281 1.228 0.4119 0.962 0.0662 1.0000 Uiso H282 1.168 0.4068 0.798 0.0662 1.0000 Uiso H283 1.065 0.3773 0.886 0.0662 1.0000 Uiso H291 1.500 0.3122 0.967 0.0662 1.0000 Uiso H292 1.482 0.2281 0.890 0.0662 1.0000 Uiso H293 1.439 0.3086 0.803 0.0662 1.0000 Uiso H321 0.4577 0.2590 0.385 0.0659 1.0000 Uiso H322 0.6032 0.2778 0.342 0.0659 1.0000 Uiso H323 0.5530 0.1874 0.352 0.0659 1.0000 Uiso H331 0.4690 0.1968 0.650 0.0658 1.0000 Uiso H332 0.6226 0.1707 0.761 0.0658 1.0000 Uiso H333 0.5586 0.1213 0.622 0.0658 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 W1 0.0263(3) 0.0480(4) 0.0302(3) 0.0052(12) 0.0129(2) 0.0012(9) N1 0.0285(9) 0.050(1) 0.032(1) 0.0049(14) 0.0116(9) 0.0016(13) N2 0.0271(9) 0.0481(9) 0.0308(9) 0.0052(14) 0.0124(8) 0.0009(12) N3 0.0268(9) 0.0483(9) 0.0306(9) 0.0054(14) 0.0124(8) 0.0012(12) N4 0.0273(8) 0.0485(9) 0.0312(9) 0.0051(14) 0.0122(8) 0.0011(12) Si1 0.039(3) 0.063(4) 0.045(3) -0.004(3) 0.007(2) -0.008(3) Si2 0.032(3) 0.070(4) 0.043(3) 0.001(3) 0.015(2) 0.008(3) C1 0.0306(12) 0.0515(13) 0.0331(13) 0.0046(17) 0.0101(12) 0.0021(15) C2 0.0312(14) 0.0520(15) 0.0336(14) 0.0045(18) 0.0097(13) 0.0022(17) C3 0.0313(14) 0.0521(15) 0.0337(15) 0.0045(18) 0.0096(13) 0.0022(17) C4 0.0313(14) 0.0520(15) 0.0337(14) 0.0045(18) 0.0095(13) 0.0023(17) C5 0.0314(14) 0.0521(15) 0.0337(15) 0.0044(18) 0.0094(13) 0.0024(17) C6 0.0313(14) 0.0520(15) 0.0336(14) 0.0045(18) 0.0096(13) 0.0022(17) C7 0.0282(9) 0.049(1) 0.031(1) 0.0051(14) 0.0115(9) 0.0016(13) C8 0.0291(12) 0.0491(12) 0.0321(12) 0.0050(16) 0.0108(11) 0.0018(14) C9 0.0293(13) 0.0492(13) 0.0323(13) 0.0050(16) 0.0107(12) 0.0017(15) C10 0.0291(12) 0.0491(13) 0.0320(12) 0.0050(16) 0.0109(11) 0.0017(14) C11 0.0293(13) 0.0492(13) 0.0322(13) 0.0050(17) 0.0108(12) 0.0018(15) C12 0.0293(13) 0.0492(14) 0.0323(13) 0.0050(17) 0.0107(12) 0.0018(15) C13 0.0282(9) 0.049(1) 0.032(1) 0.0051(15) 0.0116(9) 0.0005(13) C14 0.0290(12) 0.0493(12) 0.0321(12) 0.0050(16) 0.0111(11) 0.0002(14) C15 0.0291(12) 0.0494(13) 0.0321(12) 0.0050(16) 0.0111(12) 0.0003(15) C16 0.0290(12) 0.0494(12) 0.0321(12) 0.0050(16) 0.0111(11) 0.0003(14) C17 0.0291(12) 0.0494(13) 0.0322(12) 0.0051(16) 0.0111(12) 0.0002(15) C18 0.0289(12) 0.0493(12) 0.0321(12) 0.0050(16) 0.0112(11) 0.0003(14) C19 0.028(1) 0.0486(11) 0.031(1) 0.0050(15) 0.012(1) 0.0012(13) C20 0.028(1) 0.0487(11) 0.0315(11) 0.0050(15) 0.012(1) 0.0012(14) C21 0.028(1) 0.0487(11) 0.031(1) 0.0050(15) 0.012(1) 0.0011(13) C22 0.028(1) 0.0487(11) 0.0314(11) 0.0051(15) 0.012(1) 0.0012(14) C23 0.0276(9) 0.049(1) 0.0313(9) 0.0051(14) 0.0121(9) 0.0012(13) C24 0.0278(9) 0.049(1) 0.0313(9) 0.0052(14) 0.0121(9) 0.0012(13) C25 0.0283(13) 0.0490(14) 0.0316(13) 0.0053(17) 0.0121(13) 0.0015(16) C26 0.028(1) 0.048(1) 0.031(1) 0.0053(15) 0.012(1) 0.0010(13) C27 0.027(1) 0.049(1) 0.031(1) 0.0054(15) 0.012(1) 0.0011(13) C28 0.039(3) 0.063(4) 0.045(4) -0.004(3) 0.007(3) -0.008(3) C29 0.039(3) 0.063(4) 0.045(4) -0.004(3) 0.007(3) -0.008(3) C30 0.039(3) 0.063(4) 0.045(4) -0.004(3) 0.007(3) -0.008(3) C31 0.033(3) 0.070(5) 0.043(3) 0.001(3) 0.014(3) 0.008(3) C32 0.032(3) 0.070(5) 0.043(3) 0.001(3) 0.014(3) 0.008(3) C33 0.032(3) 0.070(5) 0.043(3) 0.001(3) 0.015(3) 0.008(3) 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 W1 . N1 . 1.771(15) yes W1 . N2 . 1.996(15) yes W1 . N3 . 2.032(15) yes W1 . N4 . 2.302(13) yes W1 . C7 . 2.199(19) yes W1 . C13 . 2.207(19) yes N1 . C1 . 1.40(2) yes N2 . Si1 . 1.787(18) yes N2 . C26 . 1.46(2) yes N3 . Si2 . 1.757(14) yes N3 . C27 . 1.48(2) yes N4 . C19 . 1.33(2) yes N4 . C23 . 1.42(2) yes Si1 . C28 . 1.92(2) yes Si1 . C29 . 1.86(2) yes Si1 . C30 . 1.84(2) yes Si2 . C31 . 1.82(3) yes Si2 . C32 . 1.91(2) yes Si2 . C33 . 1.88(2) yes C1 . C2 . 1.37(2) yes C1 . C6 . 1.40(2) yes C2 . C3 . 1.408(18) yes C3 . C4 . 1.32(2) yes C4 . C5 . 1.37(2) yes C5 . C6 . 1.38(2) yes C7 . C8 . 1.36(2) yes C7 . C12 . 1.44(3) yes C8 . C9 . 1.50(3) yes C9 . C10 . 1.36(3) yes C10 . C11 . 1.40(2) yes C11 . C12 . 1.39(3) yes C13 . C14 . 1.53(3) yes C13 . C18 . 1.30(3) yes C14 . C15 . 1.32(3) yes C15 . C16 . 1.38(3) yes C16 . C17 . 1.41(3) yes C17 . C18 . 1.48(3) yes C19 . C20 . 1.35(2) yes C20 . C21 . 1.48(2) yes C21 . C22 . 1.31(2) yes C22 . C23 . 1.38(2) yes C23 . C24 . 1.45(3) yes C24 . C25 . 1.548(16) yes