#------------------------------------------------------------------------------ #$Date: 2009-04-13 20:11:08 +0100 (Mon, 13 Apr 2009) $ #$Revision: 626 $ #$URL: svn://www.crystallography.net/cod/cif/1/1100811.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100811 _chemical_name_systematic ; [Ti2(mu-O)2(C5H4Me)2{Me3SiNC(C6H5)NCH2CH2CH2NMe2}2] ; _cell_length_a 9.3597(2) _cell_length_b 10.7886(2) _cell_length_c 12.1749(3) _cell_angle_alpha 72.8419(8) _cell_angle_beta 76.2046(8) _cell_angle_gamma 72.8192(9) _cell_volume 1106.74(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' 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' '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 ' C44 H66 N6 O2 Si2 Ti2' _chemical_formula_moiety ' C44 H66 N6 O2 Si2 Ti2' _chemical_formula_weight 838.99 _cell_measurement_reflns_used 4378 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _cell_measurement_temperature 150 _cell_formula_units_Z 1 _exptl_crystal_description 'plate ' _exptl_crystal_colour 'orange ' _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.45 _exptl_crystal_density_diffrn 1.26 _exptl_crystal_F_000 448 _exptl_absorpt_coefficient_mu 0.45 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.874 _exptl_absorpt_correction_T_max 0.914 _exptl_crystal_density_method none _exptl_crystal_density_meas 'not measured' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_reflns_av_sigmaI/netI 0.069 _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 0.71073 _diffrn_measurement_method 2\q/\w _diffrn_ambient_temperature 150 _diffrn_reflns_number 9040 _reflns_number_total 4955 _diffrn_reflns_av_R_equivalents 0.02 _reflns_number_observed 3814 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -11 _reflns_limit_h_max 12 _reflns_limit_k_min -13 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -0.31 _refine_diff_density_max 0.31 _refine_ls_number_reflns 3814 _refine_ls_number_parameters 245 _refine_ls_R_factor_obs 0.0367 _refine_ls_wR_factor_obs 0.0387 _refine_ls_goodness_of_fit_obs 1.076 _refine_ls_shift/esd_max 0.0025 _refine_ls_structure_factor_coef F _refine_ls_extinction_coef 127.4(354) _refine_ls_hydrogen_treatment 'riding model' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_hydrogens geometric _refine_ls_matrix_type full _refine_ls_weighting_scheme 'Chebychev polynomial' _refine_ls_number_restraints 0 _refine_ls_abs_structure_flack none _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_structure_solution ; CRYSTALS Issue 10 (Watkin et al, 1996) ; _computing_structure_refinement ; 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_thermal_displace_type Ti1 0.03615(3) 0.36211(3) 0.54027(3) 0.0203 1.0000 Uani N1 0.2182(2) 0.2654(1) 0.6459(1) 0.0240 1.0000 Uani N2 -0.0241(2) 0.3221(1) 0.7222(1) 0.0238 1.0000 Uani N3 -0.3255(2) 0.3319(2) 1.0535(1) 0.0307 1.0000 Uani O1 0.1359(1) 0.4893(1) 0.4595(1) 0.0237 1.0000 Uani Si1 0.41383(5) 0.24223(5) 0.62235(4) 0.0259 1.0000 Uani C1 0.1169(2) 0.2844(2) 0.7408(1) 0.0221 1.0000 Uani C2 0.1591(2) 0.2667(2) 0.8567(1) 0.0241 1.0000 Uani C3 0.1997(2) 0.1391(2) 0.9280(2) 0.0316 1.0000 Uani C4 0.2407(3) 0.1226(2) 1.0346(2) 0.0397 1.0000 Uani C5 0.2407(2) 0.2319(2) 1.0709(2) 0.0395 1.0000 Uani C6 0.2002(3) 0.3594(2) 1.0010(2) 0.0395 1.0000 Uani C7 0.1586(2) 0.3769(2) 0.8943(2) 0.0326 1.0000 Uani C8 -0.1557(2) 0.3559(2) 0.8101(2) 0.0264 1.0000 Uani C9 -0.2174(2) 0.2350(2) 0.8792(2) 0.0297 1.0000 Uani C10 -0.3531(2) 0.2662(2) 0.9741(2) 0.0297 1.0000 Uani C11 -0.4642(3) 0.3664(2) 1.1348(2) 0.0399 1.0000 Uani C12 -0.2052(3) 0.2475(2) 1.1184(2) 0.0448 1.0000 Uani C13 0.5084(3) 0.0768(2) 0.7094(2) 0.0480 1.0000 Uani C14 0.4835(2) 0.2473(3) 0.4653(2) 0.0421 1.0000 Uani C15 0.4675(2) 0.3775(2) 0.6586(2) 0.0441 1.0000 Uani C16 0.0324(3) 0.1333(2) 0.5455(2) 0.0351 1.0000 Uani C17 -0.1075(2) 0.2171(2) 0.5242(2) 0.0369 1.0000 Uani C18 -0.0900(3) 0.3104(2) 0.4196(2) 0.0455 1.0000 Uani C19 0.0606(4) 0.2870(2) 0.3726(2) 0.0513 1.0000 Uani C20 0.1397(2) 0.1776(3) 0.4496(2) 0.0477 1.0000 Uani C21 0.0639(5) 0.0204(2) 0.6490(3) 0.0774 1.0000 Uani H31 0.1997(2) 0.0628(2) 0.9028(2) 0.0424 1.0000 Uiso H41 0.2690(3) 0.0345(2) 1.0837(2) 0.0532 1.0000 Uiso H51 0.2688(2) 0.2199(2) 1.1449(2) 0.0530 1.0000 Uiso H61 0.2008(3) 0.4354(2) 1.0264(2) 0.0559 1.0000 Uiso H71 0.1291(2) 0.4653(2) 0.8462(2) 0.0464 1.0000 Uiso H81 -0.1263(2) 0.3909(2) 0.8630(2) 0.0353 1.0000 Uiso H82 -0.2341(2) 0.4226(2) 0.7722(2) 0.0353 1.0000 Uiso H91 -0.1380(2) 0.1681(2) 0.9157(2) 0.0409 1.0000 Uiso H92 -0.2475(2) 0.2010(2) 0.8260(2) 0.0409 1.0000 Uiso H101 -0.3792(2) 0.1840(2) 1.0188(2) 0.0419 1.0000 Uiso H102 -0.4367(2) 0.3241(2) 0.9367(2) 0.0419 1.0000 Uiso H111 -0.4459(3) 0.4094(2) 1.1870(2) 0.0529 1.0000 Uiso H112 -0.4968(3) 0.2869(2) 1.1788(2) 0.0529 1.0000 Uiso H113 -0.5417(3) 0.4262(2) 1.0918(2) 0.0529 1.0000 Uiso H121 -0.1900(3) 0.2936(2) 1.1694(2) 0.0602 1.0000 Uiso H122 -0.2323(3) 0.1658(2) 1.1635(2) 0.0602 1.0000 Uiso H123 -0.1134(3) 0.2274(2) 1.0644(2) 0.0602 1.0000 Uiso H131 0.6161(3) 0.0672(2) 0.6943(2) 0.0566 1.0000 Uiso H132 0.4711(3) 0.0715(2) 0.7908(2) 0.0566 1.0000 Uiso H133 0.4862(3) 0.0066(2) 0.6878(2) 0.0566 1.0000 Uiso H141 0.5917(2) 0.2347(3) 0.4492(2) 0.0550 1.0000 Uiso H142 0.4372(2) 0.3323(3) 0.4192(2) 0.0550 1.0000 Uiso H143 0.4573(2) 0.1774(3) 0.4463(2) 0.0550 1.0000 Uiso H151 0.5759(2) 0.3623(2) 0.6448(2) 0.0641 1.0000 Uiso H152 0.4291(2) 0.3777(2) 0.7391(2) 0.0641 1.0000 Uiso H153 0.4248(2) 0.4623(2) 0.6103(2) 0.0641 1.0000 Uiso H171 -0.2022(2) 0.2102(2) 0.5747(2) 0.0543 1.0000 Uiso H181 -0.1698(3) 0.3801(2) 0.3862(2) 0.0635 1.0000 Uiso H191 0.1049(4) 0.3364(2) 0.2995(2) 0.0658 1.0000 Uiso H201 0.2471(2) 0.1395(3) 0.4392(2) 0.0685 1.0000 Uiso H211 0.1707(5) -0.0202(2) 0.6413(3) 0.0858 1.0000 Uiso H212 0.0311(5) 0.0532(2) 0.7184(3) 0.0858 1.0000 Uiso H213 0.0100(5) -0.0448(2) 0.6540(3) 0.0858 1.0000 Uiso