Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_letter ; These are the CIF format data (4 structures) for the paper Imido titanium compounds bearing the 6-dimethylamino-1,4,6- trimethyl-1,4-diazacycloheptane ligand: synthesis, structures solution dynamics and ethylene polymerisation capability Gregory J Hayday, Chao Wang, Nicholas H Rees and Philip Mountford ; _publ_contact_author ; Professor P Mountford Chemistry Reaearch Laboratory Mansfield Road Oxford OX1 3TA UK ; _publ_contact_author_phone '+44 1865 285140' _publ_contact_author_fax '+44 1865 285141' _publ_contact_author_email PHILIP.MOUNTFORD@CHEMISTRY.OXFORD.AC.UK _publ_section_title ;Imido titanium compounds bearing the 6-dimethylamino-1,4,6-trimethyl-1,4-diazacycloheptane ligand: synthesis, structures, solution dynamics and ethylene polymerisation capability ; _publ_contact_author_name 'Prof. Philip Mountford' loop_ _publ_author_name 'Gregory J. Hayday' 'Chao Wang.' 'Nicholas H. Rees' 'Philip Mountford' data_COMPOUND_1-trans _database_code_depnum_ccdc_archive 'CCDC 676927' # Local code CW4a _chemical_name_systematic ; Ti(NtBu)(Me4DACH)Cl2 ; _publ_section_exptl_refinement ; No special details ; _chemical_melting_point ? _cell_length_a 7.6347(3) _cell_length_b 11.2775(6) _cell_length_c 22.2136(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1912.60(15) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P c m n ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y,z+1/2 x+1/2,-y,-z+1/2 x,-y+1/2,z -x,y+1/2,-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 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' Ti 0.2776 0.4457 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C14 H32 Cl2 N4 Ti1' _chemical_formula_moiety 'C14 H32 Cl2 N4 Ti1' _chemical_compound_source ? _chemical_formula_weight 375.24 _cell_measurement_reflns_used 94050 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_min 0.03 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_meas ? _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 0.727 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.97 _exptl_absorpt_correction_T_max 0.98 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 6496 _reflns_number_total 2259 _diffrn_reflns_av_R_equivalents 0.109 _diffrn_reflns_theta_min 5.153 _diffrn_reflns_theta_max 27.493 _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 26.393 _diffrn_measured_fraction_theta_full 0.983 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _reflns_limit_h_min 0 _reflns_limit_h_max 9 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _oxford_diffrn_Wilson_B_factor 2.20 _oxford_diffrn_Wilson_scale 5.84 _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.10 _refine_diff_density_max 0.62 _refine_ls_extinction_method None _refine_ls_number_reflns 1595 _refine_ls_number_restraints 4 _refine_ls_number_parameters 108 _refine_ls_wR_factor_ref 0.0602 _refine_ls_goodness_of_fit_ref 1.0552 _refine_ls_R_factor_all 0.0827 _refine_ls_wR_factor_all 0.0671 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 1595 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_gt 0.0602 _refine_ls_shift/su_max 0.000821 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 2.01 0.979 1.69 ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. 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_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ti1 Ti 0.16987(8) 0.2500 0.36802(3) 0.0210 1.0000 Uani S T . . . . Cl1 Cl -0.02385(8) 0.09012(6) 0.34456(3) 0.0320 1.0000 Uani . . . . . . N1 N 0.2606(4) 0.2500 0.26028(14) 0.0236 1.0000 Uani S T . . . . N2 N 0.4122(3) 0.3671(2) 0.36490(11) 0.0282 1.0000 Uani . . . . . . N3 N 0.1492(4) 0.2500 0.44429(14) 0.0253 1.0000 Uani S T . . . . C1 C 0.4563(5) 0.2500 0.26969(17) 0.0284 1.0000 Uani S T . . . . C2 C 0.5029(3) 0.3608(3) 0.30477(13) 0.0323 1.0000 Uani . . . . . . C3 C 0.5299(4) 0.3181(3) 0.41223(14) 0.0362 1.0000 Uani . . . . . . C4 C 0.5650(5) 0.250000(7) 0.2109(2) 0.0350 1.0000 Uani S T . . . . C5 C 0.1992(4) 0.1458(3) 0.22579(13) 0.0340 1.0000 Uani . . . . . . C6 C 0.3803(4) 0.4938(3) 0.38025(14) 0.0385 1.0000 Uani . . . . . . C7 C 0.1046(6) 0.2500 0.50745(18) 0.0343 1.0000 Uani S T . . . . C8 C -0.0918(7) 0.250000(7) 0.5141(2) 0.0716 1.0000 Uani S T . . . . C9 C 0.1807(9) 0.3593(6) 0.5375(2) 0.0982 1.0000 Uani . . . . . . H21 H 0.6324 0.3628 0.3114 0.0374 1.0000 Uiso R . . . . . H22 H 0.4669 0.4313 0.2804 0.0374 1.0000 Uiso R . . . . . H31 H 0.4893 0.3468 0.4525 0.0434 1.0000 Uiso R . . . . . H32 H 0.6519 0.3468 0.4047 0.0434 1.0000 Uiso R . . . . . H41 H 0.6927 0.2500 0.2208 0.0431 1.0000 Uiso RS . . . . . H42 H 0.5360 0.3224 0.1869 0.0431 1.0000 Uiso R . . . . . H51 H 0.0692 0.1501 0.2210 0.0444 1.0000 Uiso R . . . . . H52 H 0.2310 0.0715 0.2478 0.0444 1.0000 Uiso R . . . . . H53 H 0.2559 0.1455 0.1852 0.0444 1.0000 Uiso R . . . . . H61 H 0.3204 0.4983 0.4202 0.0472 1.0000 Uiso R . . . . . H62 H 0.4943 0.5373 0.3822 0.0472 1.0000 Uiso R . . . . . H63 H 0.3041 0.5306 0.3488 0.0472 1.0000 Uiso R . . . . . H81 H -0.1254 0.2500 0.5576 0.0921 1.0000 Uiso RS . . . . . H82 H -0.1403 0.3224 0.4942 0.0921 1.0000 Uiso R . . . . . H91 H 0.1495 0.3593 0.5813 0.1139 1.0000 Uiso R . . . . . H92 H 0.3111 0.3591 0.5331 0.1139 1.0000 Uiso R . . . . . H93 H 0.1315 0.4319 0.5180 0.1139 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0183(3) 0.0174(3) 0.0274(3) 0.0000 -0.0010(2) 0.0000 Cl1 0.0277(3) 0.0250(4) 0.0433(4) -0.0024(3) 0.0013(2) -0.0079(2) N1 0.0235(14) 0.0185(13) 0.0288(14) 0.0000 -0.0028(12) 0.0000 N2 0.0247(11) 0.0225(11) 0.0373(11) -0.0036(9) -0.0002(9) -0.0059(9) N3 0.0260(14) 0.0225(14) 0.0272(14) 0.0000 0.0004(12) 0.0000 C1 0.0201(15) 0.034(2) 0.0316(19) 0.0000 0.0032(13) 0.0000 C2 0.0277(13) 0.0347(15) 0.0345(14) 0.0000(11) 0.0021(10) -0.0077(10) C3 0.0268(12) 0.0483(19) 0.0337(14) -0.0047(12) -0.0059(11) -0.0046(12) C4 0.0264(17) 0.040(2) 0.039(2) 0.0000 0.0075(16) 0.0000 C5 0.0315(13) 0.0332(14) 0.0373(14) -0.0122(11) -0.0018(11) -0.0059(11) C6 0.0423(15) 0.0237(14) 0.0496(18) -0.0098(11) 0.0048(13) -0.0085(12) C7 0.0333(19) 0.042(2) 0.0272(18) 0.0000 -0.0030(15) 0.0000 C8 0.040(3) 0.138(7) 0.036(3) 0.0000 0.007(2) 0.0000 C9 0.136(5) 0.106(4) 0.052(2) -0.044(3) 0.029(3) -0.059(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 Ti1 . N2 5_555 2.274(2) yes Ti1 . Cl1 5_555 2.3895(7) yes Ti1 . Cl1 . 2.3895(7) yes Ti1 . N1 . 2.491(3) yes Ti1 . N2 . 2.274(2) yes Ti1 . N3 . 1.702(3) yes N1 . C5 5_555 1.478(3) yes N1 . C1 . 1.509(4) yes N1 . C5 . 1.478(3) yes N2 . C2 . 1.506(4) yes N2 . C3 . 1.490(4) yes N2 . C6 . 1.488(3) yes N3 . C7 . 1.444(5) yes C1 . C2 5_555 1.515(4) yes C1 . C2 . 1.515(4) yes C1 . C4 . 1.547(5) yes C2 . H21 . 1.000 no C2 . H22 . 1.000 no C3 . C3 5_555 1.535(7) yes C3 . H31 . 1.000 no C3 . H32 . 1.000 no C4 . H42 5_555 1.000 no C4 . H41 . 1.000 no C4 . H42 . 1.000 no C5 . H51 . 1.000 no C5 . H52 . 1.000 no C5 . H53 . 1.000 no C6 . H61 . 1.000 no C6 . H62 . 1.000 no C6 . H63 . 1.000 no C7 . C9 5_555 1.518(5) yes C7 . C8 . 1.507(7) yes C7 . C9 . 1.518(5) yes C8 . H82 5_555 1.000 no C8 . H81 . 1.000 no C8 . H82 . 1.000 no C9 . H91 . 1.000 no C9 . H92 . 1.000 no C9 . H93 . 1.000 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 N2 5_555 Ti1 . Cl1 5_555 159.25(7) yes N2 5_555 Ti1 . Cl1 . 93.36(6) yes Cl1 5_555 Ti1 . Cl1 . 97.98(4) yes N2 5_555 Ti1 . N1 . 75.21(8) yes Cl1 5_555 Ti1 . N1 . 87.85(5) yes Cl1 . Ti1 . N1 . 87.85(5) yes N2 5_555 Ti1 . N2 . 71.02(12) yes Cl1 5_555 Ti1 . N2 . 93.36(6) yes Cl1 . Ti1 . N2 . 159.25(7) yes N1 . Ti1 . N2 . 75.21(8) yes N2 5_555 Ti1 . N3 . 96.07(11) yes Cl1 5_555 Ti1 . N3 . 99.19(7) yes Cl1 . Ti1 . N3 . 99.19(7) yes N1 . Ti1 . N3 . 169.18(12) yes N2 . Ti1 . N3 . 96.07(11) yes C5 5_555 N1 . Ti1 . 114.19(17) yes C5 5_555 N1 . C1 . 112.7(2) yes Ti1 . N1 . C1 . 98.2(2) yes C5 5_555 N1 . C5 . 105.2(3) yes Ti1 . N1 . C5 . 114.19(17) yes C1 . N1 . C5 . 112.7(2) yes Ti1 . N2 . C2 . 111.95(15) yes Ti1 . N2 . C3 . 104.68(17) yes C2 . N2 . C3 . 109.3(2) yes Ti1 . N2 . C6 . 114.67(17) yes C2 . N2 . C6 . 108.9(2) yes C3 . N2 . C6 . 107.0(2) yes Ti1 . N3 . C7 . 171.7(3) yes C2 5_555 C1 . N1 . 107.7(2) yes C2 5_555 C1 . C2 . 111.1(3) yes N1 . C1 . C2 . 107.7(2) yes C2 5_555 C1 . C4 . 107.9(2) yes N1 . C1 . C4 . 114.5(3) yes C2 . C1 . C4 . 107.9(2) yes C1 . C2 . N2 . 112.8(2) yes C1 . C2 . H21 . 109.0 no N2 . C2 . H21 . 108.9 no C1 . C2 . H22 . 108.2 no N2 . C2 . H22 . 108.4 no H21 . C2 . H22 . 109.5 no C3 5_555 C3 . N2 . 111.80(15) yes C3 5_555 C3 . H31 . 108.9 no N2 . C3 . H31 . 108.9 no C3 5_555 C3 . H32 . 108.9 no N2 . C3 . H32 . 108.9 no H31 . C3 . H32 . 109.5 no C1 . C4 . H42 5_555 109.4 no C1 . C4 . H41 . 109.7 no H42 5_555 C4 . H41 . 109.5 no C1 . C4 . H42 . 109.4 no H42 5_555 C4 . H42 . 109.5 no H41 . C4 . H42 . 109.5 no N1 . C5 . H51 . 109.3 no N1 . C5 . H52 . 109.6 no H51 . C5 . H52 . 109.5 no N1 . C5 . H53 . 109.4 no H51 . C5 . H53 . 109.5 no H52 . C5 . H53 . 109.5 no N2 . C6 . H61 . 109.1 no N2 . C6 . H62 . 109.8 no H61 . C6 . H62 . 109.5 no N2 . C6 . H63 . 109.5 no H61 . C6 . H63 . 109.5 no H62 . C6 . H63 . 109.5 no C9 5_555 C7 . N3 . 109.7(3) yes C9 5_555 C7 . C8 . 109.7(3) yes N3 . C7 . C8 . 109.3(4) yes C9 5_555 C7 . C9 . 108.6(6) yes N3 . C7 . C9 . 109.7(3) yes C8 . C7 . C9 . 109.7(3) yes C7 . C8 . H82 5_555 109.0 no C7 . C8 . H81 . 110.5 no H82 5_555 C8 . H81 . 109.5 no C7 . C8 . H82 . 109.0 no H82 5_555 C8 . H82 . 109.5 no H81 . C8 . H82 . 109.5 no C7 . C9 . H91 . 109.6 no C7 . C9 . H92 . 109.6 no H91 . C9 . H92 . 109.5 no C7 . C9 . H93 . 109.2 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no #===end data_COMPOUND_2-cis _database_code_depnum_ccdc_archive 'CCDC 676928' # Local code CW7 _chemical_name_systematic ; Ti(N-2,6,-C6H3Me2)(Me4DACH)Cl2 ; _publ_section_exptl_refinement ; No special details ; _chemical_melting_point ? _cell_length_a 12.1817(2) _cell_length_b 15.2253(2) _cell_length_c 15.2192(3) _cell_angle_alpha 90 _cell_angle_beta 106.8996(6) _cell_angle_gamma 90 _cell_volume 2700.81(8) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-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 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' Ti 0.2776 0.4457 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C20 H36 Cl6 N4 Ti1' _chemical_formula_moiety 'C20 H36 Cl6 N4 Ti1' _chemical_compound_source ? _chemical_formula_weight 593.15 _cell_measurement_reflns_used 6207 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.18 _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_meas ? _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 0.927 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 0.89 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 11656 _reflns_number_total 6117 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_theta_min 5.174 _diffrn_reflns_theta_max 27.444 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.895 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _oxford_diffrn_Wilson_B_factor 2.52 _oxford_diffrn_Wilson_scale 14.71 _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.39 _refine_diff_density_max 0.34 _refine_ls_number_reflns 3948 _refine_ls_number_restraints 0 _refine_ls_number_parameters 280 _refine_ls_wR_factor_ref 0.0383 _refine_ls_goodness_of_fit_ref 1.0774 _refine_ls_R_factor_all 0.0615 _refine_ls_wR_factor_all 0.0616 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 3948 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_gt 0.0383 _refine_ls_shift/su_max 0.000894 _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.439 0.211 0.224 ; 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_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ti1 Ti 0.87341(3) 0.28884(3) 0.68422(3) 0.0185 1.0000 Uani . . . . . . Cl1 Cl 0.99211(5) 0.17359(4) 0.65511(4) 0.0303 1.0000 Uani . . . . . . Cl2 Cl 0.92555(5) 0.39083(4) 0.58407(4) 0.0291 1.0000 Uani . . . . . . N1 N 0.79843(16) 0.39453(13) 0.75687(13) 0.0233 1.0000 Uani . . . . . . N2 N 1.03934(16) 0.33977(13) 0.80281(13) 0.0245 1.0000 Uani . . . . . . N3 N 0.88098(17) 0.22707(13) 0.82528(13) 0.0250 1.0000 Uani . . . . . . N4 N 0.74460(16) 0.25314(12) 0.61130(12) 0.0215 1.0000 Uani . . . . . . C1 C 0.8713(2) 0.38775(16) 0.85580(15) 0.0251 1.0000 Uani . . . . . . C2 C 0.9965(2) 0.40294(17) 0.85903(16) 0.0278 1.0000 Uani . . . . . . C3 C 1.0902(2) 0.26150(18) 0.85879(17) 0.0324 1.0000 Uani . . . . . . C4 C 1.0005(2) 0.19477(17) 0.86686(18) 0.0331 1.0000 Uani . . . . . . C5 C 0.8557(2) 0.29528(16) 0.88792(16) 0.0283 1.0000 Uani . . . . . . C6 C 0.8412(2) 0.45416(19) 0.92076(18) 0.0361 1.0000 Uani . . . . . . C7 C 0.6750(2) 0.37421(19) 0.74659(18) 0.0339 1.0000 Uani . . . . . . C8 C 0.7990(2) 0.48507(16) 0.72041(18) 0.0338 1.0000 Uani . . . . . . C9 C 1.1325(2) 0.3820(2) 0.77394(18) 0.0351 1.0000 Uani . . . . . . C10 C 0.8036(3) 0.15083(18) 0.82055(19) 0.0373 1.0000 Uani . . . . . . C11 C 0.65125(18) 0.22545(15) 0.54051(15) 0.0218 1.0000 Uani . . . . . . C12 C 0.62771(19) 0.13468(16) 0.52549(16) 0.0245 1.0000 Uani . . . . . . C13 C 0.5362(2) 0.10823(18) 0.45179(17) 0.0312 1.0000 Uani . . . . . . C14 C 0.4659(2) 0.1684(2) 0.39346(17) 0.0351 1.0000 Uani . . . . . . C15 C 0.4892(2) 0.25719(19) 0.40762(17) 0.0319 1.0000 Uani . . . . . . C16 C 0.58103(19) 0.28726(16) 0.47925(16) 0.0260 1.0000 Uani . . . . . . C17 C 0.7007(2) 0.06674(16) 0.58810(17) 0.0289 1.0000 Uani . . . . . . C18 C 0.6042(2) 0.38412(17) 0.48972(18) 0.0339 1.0000 Uani . . . . . . H21 H 1.0453 0.3980 0.9242 0.0327 1.0000 Uiso R . . . . . H22 H 1.0033 0.4636 0.8359 0.0327 1.0000 Uiso R . . . . . H31 H 1.1338 0.2814 0.9219 0.0361 1.0000 Uiso R . . . . . H32 H 1.1439 0.2326 0.8290 0.0361 1.0000 Uiso R . . . . . H41 H 1.0117 0.1818 0.9333 0.0388 1.0000 Uiso R . . . . . H42 H 1.0112 0.1397 0.8345 0.0388 1.0000 Uiso R . . . . . H51 H 0.9085 0.2864 0.9512 0.0342 1.0000 Uiso R . . . . . H52 H 0.7744 0.2883 0.8889 0.0342 1.0000 Uiso R . . . . . H61 H 0.8926 0.4455 0.9846 0.0452 1.0000 Uiso R . . . . . H62 H 0.8512 0.5151 0.8997 0.0452 1.0000 Uiso R . . . . . H63 H 0.7595 0.4454 0.9200 0.0452 1.0000 Uiso R . . . . . H71 H 0.6295 0.3793 0.6805 0.0426 1.0000 Uiso R . . . . . H72 H 0.6448 0.4168 0.7840 0.0426 1.0000 Uiso R . . . . . H73 H 0.6684 0.3131 0.7686 0.0426 1.0000 Uiso R . . . . . H81 H 0.7504 0.4872 0.6550 0.0409 1.0000 Uiso R . . . . . H82 H 0.8795 0.5021 0.7240 0.0409 1.0000 Uiso R . . . . . H83 H 0.7679 0.5269 0.7579 0.0409 1.0000 Uiso R . . . . . H91 H 1.1621 0.3401 0.7356 0.0431 1.0000 Uiso R . . . . . H92 H 1.1962 0.3990 0.8293 0.0431 1.0000 Uiso R . . . . . H93 H 1.1018 0.4357 0.7371 0.0431 1.0000 Uiso R . . . . . H101 H 0.7223 0.1700 0.7930 0.0465 1.0000 Uiso R . . . . . H102 H 0.8134 0.1274 0.8838 0.0465 1.0000 Uiso R . . . . . H103 H 0.8228 0.1038 0.7815 0.0465 1.0000 Uiso R . . . . . H131 H 0.5208 0.0441 0.4406 0.0365 1.0000 Uiso R . . . . . H141 H 0.3994 0.1481 0.3419 0.0411 1.0000 Uiso R . . . . . H151 H 0.4388 0.3008 0.3655 0.0370 1.0000 Uiso R . . . . . H171 H 0.6714 0.0066 0.5671 0.0347 1.0000 Uiso R . . . . . H172 H 0.6972 0.0764 0.6523 0.0347 1.0000 Uiso R . . . . . H173 H 0.7819 0.0723 0.5865 0.0347 1.0000 Uiso R . . . . . H181 H 0.5459 0.4163 0.4403 0.0396 1.0000 Uiso R . . . . . H182 H 0.5991 0.4036 0.5512 0.0396 1.0000 Uiso R . . . . . H183 H 0.6827 0.3969 0.4847 0.0396 1.0000 Uiso R . . . . . C101 C 0.5968(3) 0.6961(2) 0.8659(3) 0.0501 1.0000 Uani . . . . . . Cl101 Cl 0.74160(6) 0.69884(5) 0.86568(6) 0.0458 1.0000 Uani . . . . . . Cl102 Cl 0.52480(7) 0.60620(5) 0.80165(6) 0.0487 1.0000 Uani . . . . . . H1011 H 0.5935 0.6908 0.9306 0.0645 1.0000 Uiso R . . . . . H1012 H 0.5582 0.7517 0.8382 0.0645 1.0000 Uiso R . . . . . C201 C 0.2336(2) 0.42788(19) 0.56473(18) 0.0355 1.0000 Uani . . . . . . Cl201 Cl 0.33734(6) 0.44726(5) 0.67156(4) 0.0409 1.0000 Uani . . . . . . Cl202 Cl 0.29717(7) 0.37964(5) 0.48673(5) 0.0418 1.0000 Uani . . . . . . H2011 H 0.1973 0.4849 0.5391 0.0412 1.0000 Uiso R . . . . . H2012 H 0.1736 0.3873 0.5744 0.0412 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.01895(18) 0.0202(2) 0.01600(18) -0.00068(15) 0.00458(14) -0.00166(15) Cl1 0.0260(3) 0.0321(3) 0.0319(3) -0.0066(2) 0.0067(2) 0.0050(2) Cl2 0.0310(3) 0.0342(3) 0.0232(3) 0.0053(2) 0.0095(2) -0.0051(2) N1 0.0245(9) 0.0235(10) 0.0220(9) -0.0023(8) 0.0071(7) -0.0011(8) N2 0.0240(9) 0.0280(10) 0.0212(9) -0.0011(8) 0.0061(7) -0.0012(8) N3 0.0317(10) 0.0220(10) 0.0201(9) 0.0019(7) 0.0056(8) -0.0052(8) N4 0.0231(9) 0.0204(9) 0.0208(9) -0.0001(7) 0.0060(7) -0.0017(7) C1 0.0293(12) 0.0282(12) 0.0197(11) -0.0050(9) 0.0099(9) -0.0020(10) C2 0.0285(12) 0.0286(12) 0.0243(11) -0.0071(10) 0.0046(9) -0.0055(10) C3 0.0283(12) 0.0353(14) 0.0266(12) 0.0001(10) -0.0030(10) 0.0063(10) C4 0.0406(14) 0.0311(13) 0.0248(12) 0.0076(10) 0.0052(10) 0.0065(11) C5 0.0350(13) 0.0327(13) 0.0192(11) 0.0007(10) 0.0111(9) -0.0045(11) C6 0.0423(15) 0.0387(15) 0.0301(13) -0.0094(11) 0.0150(11) -0.0009(12) C7 0.0248(12) 0.0459(16) 0.0325(13) -0.0036(12) 0.0108(10) 0.0016(11) C8 0.0471(15) 0.0253(13) 0.0294(13) 0.0014(10) 0.0116(11) 0.0049(11) C9 0.0216(11) 0.0490(16) 0.0339(13) -0.0042(12) 0.0069(10) -0.0114(11) C10 0.0528(16) 0.0306(14) 0.0291(13) 0.0017(11) 0.0130(12) -0.0152(12) C11 0.0189(10) 0.0284(12) 0.0191(10) -0.0021(9) 0.0071(8) -0.0037(9) C12 0.0249(11) 0.0272(12) 0.0236(11) -0.0038(9) 0.0103(9) -0.0044(9) C13 0.0293(12) 0.0341(14) 0.0299(12) -0.0104(10) 0.0082(10) -0.0096(10) C14 0.0272(13) 0.0495(16) 0.0252(12) -0.0067(12) 0.0022(10) -0.0088(11) C15 0.0259(12) 0.0443(15) 0.0231(12) 0.0030(11) 0.0032(9) 0.0006(11) C16 0.0228(11) 0.0315(13) 0.0234(11) 0.0001(10) 0.0065(9) -0.0033(10) C17 0.0310(12) 0.0271(12) 0.0294(12) -0.0040(10) 0.0102(10) -0.0039(10) C18 0.0347(13) 0.0297(13) 0.0314(13) 0.0059(10) 0.0004(10) -0.0027(11) C101 0.0392(16) 0.0476(18) 0.070(2) -0.0186(16) 0.0265(15) -0.0083(13) Cl101 0.0355(4) 0.0395(4) 0.0659(5) -0.0108(3) 0.0204(3) -0.0037(3) Cl102 0.0457(4) 0.0530(4) 0.0507(4) -0.0072(3) 0.0192(3) -0.0163(3) C201 0.0353(14) 0.0351(14) 0.0346(14) 0.0012(11) 0.0076(11) 0.0009(11) Cl201 0.0481(4) 0.0411(4) 0.0308(3) 0.0006(3) 0.0074(3) -0.0086(3) Cl202 0.0558(4) 0.0368(4) 0.0352(3) -0.0030(3) 0.0171(3) -0.0034(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2251(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 Ti1 . Cl1 . 2.3956(7) yes Ti1 . Cl2 . 2.3876(7) yes Ti1 . N1 . 2.2876(19) yes Ti1 . N2 . 2.4132(19) yes Ti1 . N3 . 2.3210(19) yes Ti1 . N4 . 1.7253(19) yes N1 . C1 . 1.513(3) yes N1 . C7 . 1.498(3) yes N1 . C8 . 1.487(3) yes N2 . C2 . 1.480(3) yes N2 . C3 . 1.491(3) yes N2 . C9 . 1.477(3) yes N3 . C4 . 1.493(3) yes N3 . C5 . 1.501(3) yes N3 . C10 . 1.484(3) yes N4 . C11 . 1.385(3) yes C1 . C2 . 1.529(3) yes C1 . C5 . 1.520(3) yes C1 . C6 . 1.532(3) yes C2 . H21 . 1.000 no C2 . H22 . 1.000 no C3 . C4 . 1.522(4) yes C3 . H31 . 1.000 no C3 . H32 . 1.000 no C4 . H41 . 1.000 no C4 . H42 . 1.000 no C5 . H51 . 1.000 no C5 . H52 . 1.000 no C6 . H61 . 1.000 no C6 . H62 . 1.000 no C6 . H63 . 1.000 no C7 . H71 . 1.000 no C7 . H72 . 1.000 no C7 . H73 . 1.000 no C8 . H81 . 1.000 no C8 . H82 . 1.000 no C8 . H83 . 1.000 no C9 . H91 . 1.000 no C9 . H92 . 1.000 no C9 . H93 . 1.000 no C10 . H101 . 1.000 no C10 . H102 . 1.000 no C10 . H103 . 1.000 no C11 . C12 . 1.417(3) yes C11 . C16 . 1.422(3) yes C12 . C13 . 1.392(3) yes C12 . C17 . 1.508(3) yes C13 . C14 . 1.385(4) yes C13 . H131 . 1.000 no C14 . C15 . 1.385(4) yes C14 . H141 . 1.000 no C15 . C16 . 1.393(3) yes C15 . H151 . 1.000 no C16 . C18 . 1.501(3) yes C17 . H171 . 1.000 no C17 . H172 . 1.000 no C17 . H173 . 1.000 no C18 . H181 . 1.000 no C18 . H182 . 1.000 no C18 . H183 . 1.000 no C101 . Cl101 . 1.765(3) yes C101 . Cl102 . 1.761(3) yes C101 . H1011 . 1.000 no C101 . H1012 . 1.000 no C201 . Cl201 . 1.770(3) yes C201 . Cl202 . 1.755(3) yes C201 . H2011 . 1.000 no C201 . H2012 . 1.000 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 Cl1 . Ti1 . Cl2 . 94.10(3) yes Cl1 . Ti1 . N1 . 162.16(5) yes Cl2 . Ti1 . N1 . 93.94(5) yes Cl1 . Ti1 . N2 . 87.38(5) yes Cl2 . Ti1 . N2 . 87.02(5) yes N1 . Ti1 . N2 . 77.16(7) yes Cl1 . Ti1 . N3 . 90.60(5) yes Cl2 . Ti1 . N3 . 155.18(5) yes N1 . Ti1 . N3 . 75.64(7) yes N2 . Ti1 . N3 . 68.84(7) yes Cl1 . Ti1 . N4 . 97.77(7) yes Cl2 . Ti1 . N4 . 98.93(6) yes N1 . Ti1 . N4 . 96.68(8) yes N2 . Ti1 . N4 . 171.78(8) yes N3 . Ti1 . N4 . 104.56(8) yes Ti1 . N1 . C1 . 103.40(13) yes Ti1 . N1 . C7 . 109.50(15) yes C1 . N1 . C7 . 111.75(18) yes Ti1 . N1 . C8 . 115.21(14) yes C1 . N1 . C8 . 111.69(18) yes C7 . N1 . C8 . 105.4(2) yes Ti1 . N2 . C2 . 106.37(13) yes Ti1 . N2 . C3 . 106.80(14) yes C2 . N2 . C3 . 110.30(19) yes Ti1 . N2 . C9 . 117.77(14) yes C2 . N2 . C9 . 108.64(19) yes C3 . N2 . C9 . 106.9(2) yes Ti1 . N3 . C4 . 107.28(14) yes Ti1 . N3 . C5 . 110.29(14) yes C4 . N3 . C5 . 108.28(19) yes Ti1 . N3 . C10 . 114.72(15) yes C4 . N3 . C10 . 106.9(2) yes C5 . N3 . C10 . 109.13(19) yes Ti1 . N4 . C11 . 169.58(16) yes N1 . C1 . C2 . 108.23(18) yes N1 . C1 . C5 . 106.94(18) yes C2 . C1 . C5 . 110.3(2) yes N1 . C1 . C6 . 114.6(2) yes C2 . C1 . C6 . 107.7(2) yes C5 . C1 . C6 . 109.2(2) yes C1 . C2 . N2 . 113.53(19) yes C1 . C2 . H21 . 108.7 no N2 . C2 . H21 . 108.4 no C1 . C2 . H22 . 108.2 no N2 . C2 . H22 . 108.5 no H21 . C2 . H22 . 109.5 no N2 . C3 . C4 . 113.0(2) yes N2 . C3 . H31 . 108.8 no C4 . C3 . H31 . 108.6 no N2 . C3 . H32 . 108.1 no C4 . C3 . H32 . 108.8 no H31 . C3 . H32 . 109.5 no C3 . C4 . N3 . 112.4(2) yes C3 . C4 . H41 . 108.9 no N3 . C4 . H41 . 108.8 no C3 . C4 . H42 . 108.7 no N3 . C4 . H42 . 108.5 no H41 . C4 . H42 . 109.5 no C1 . C5 . N3 . 111.64(18) yes C1 . C5 . H51 . 109.3 no N3 . C5 . H51 . 109.0 no C1 . C5 . H52 . 108.6 no N3 . C5 . H52 . 108.8 no H51 . C5 . H52 . 109.5 no C1 . C6 . H61 . 109.9 no C1 . C6 . H62 . 109.3 no H61 . C6 . H62 . 109.5 no C1 . C6 . H63 . 109.2 no H61 . C6 . H63 . 109.5 no H62 . C6 . H63 . 109.5 no N1 . C7 . H71 . 109.6 no N1 . C7 . H72 . 109.3 no H71 . C7 . H72 . 109.5 no N1 . C7 . H73 . 109.5 no H71 . C7 . H73 . 109.5 no H72 . C7 . H73 . 109.5 no N1 . C8 . H81 . 109.6 no N1 . C8 . H82 . 109.3 no H81 . C8 . H82 . 109.5 no N1 . C8 . H83 . 109.5 no H81 . C8 . H83 . 109.5 no H82 . C8 . H83 . 109.5 no N2 . C9 . H91 . 109.5 no N2 . C9 . H92 . 109.7 no H91 . C9 . H92 . 109.5 no N2 . C9 . H93 . 109.2 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no N3 . C10 . H101 . 109.3 no N3 . C10 . H102 . 109.6 no H101 . C10 . H102 . 109.5 no N3 . C10 . H103 . 109.5 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no N4 . C11 . C12 . 120.3(2) yes N4 . C11 . C16 . 120.7(2) yes C12 . C11 . C16 . 119.0(2) yes C11 . C12 . C13 . 119.3(2) yes C11 . C12 . C17 . 120.8(2) yes C13 . C12 . C17 . 119.8(2) yes C12 . C13 . C14 . 121.7(2) yes C12 . C13 . H131 . 119.1 no C14 . C13 . H131 . 119.1 no C13 . C14 . C15 . 119.1(2) yes C13 . C14 . H141 . 120.5 no C15 . C14 . H141 . 120.5 no C14 . C15 . C16 . 121.6(2) yes C14 . C15 . H151 . 119.2 no C16 . C15 . H151 . 119.2 no C11 . C16 . C15 . 119.3(2) yes C11 . C16 . C18 . 121.4(2) yes C15 . C16 . C18 . 119.3(2) yes C12 . C17 . H171 . 109.6 no C12 . C17 . H172 . 109.4 no H171 . C17 . H172 . 109.5 no C12 . C17 . H173 . 109.4 no H171 . C17 . H173 . 109.5 no H172 . C17 . H173 . 109.5 no C16 . C18 . H181 . 109.4 no C16 . C18 . H182 . 109.3 no H181 . C18 . H182 . 109.5 no C16 . C18 . H183 . 109.8 no H181 . C18 . H183 . 109.5 no H182 . C18 . H183 . 109.5 no Cl101 . C101 . Cl102 . 110.76(17) yes Cl101 . C101 . H1011 . 109.3 no Cl102 . C101 . H1011 . 109.2 no Cl101 . C101 . H1012 . 109.1 no Cl102 . C101 . H1012 . 109.0 no H1011 . C101 . H1012 . 109.5 no Cl201 . C201 . Cl202 . 110.71(15) yes Cl201 . C201 . H2011 . 109.3 no Cl202 . C201 . H2011 . 109.4 no Cl201 . C201 . H2012 . 109.0 no Cl202 . C201 . H2012 . 109.0 no H2011 . C201 . H2012 . 109.5 no #===end data_COMPOUND_3-trans _database_code_depnum_ccdc_archive 'CCDC 676929' # Local code ADSCW 18 _chemical_name_systematic ; Ti(N-2,6-C6H3iPr2)(Me4DACH)Cl2 .CH2Cl2 ; _chemical_melting_point ? _publ_section_exptl_refinement ; The titanium complex and the CH2Cl2 crystallisation lie across crystallographic mirror planes at y = 1/4. The CH2Cl2 is slightly disordered across this mirror plane. H atoms were placed in calculated positions and refined in a riding model. ; _cell_length_a 9.3464(2) _cell_length_b 13.9957(3) _cell_length_c 21.1047(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2760.69(11) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P c m n ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y,z+1/2 x+1/2,-y,-z+1/2 x,-y+1/2,z -x,y+1/2,-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 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' Ti 0.2776 0.4457 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C23 H42 Cl4 N4 Ti1' _chemical_formula_moiety 'C22 H40 Cl4 N4 Ti1, CH2Cl2' _chemical_compound_source ? _chemical_formula_weight 564.32 _cell_measurement_reflns_used 5808 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 0.716 # Sheldrick geometric approximatio 0.81 0.87 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.87 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 11674 _reflns_number_total 3261 _diffrn_reflns_av_R_equivalents 0.037 # Number of reflections with Friedels Law is 3261 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 3169 _diffrn_reflns_theta_min 5.238 _diffrn_reflns_theta_max 27.493 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.493 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _reflns_limit_h_min 0 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 27 _oxford_diffrn_Wilson_B_factor 1.85 _oxford_diffrn_Wilson_scale 18.25 _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.33 _refine_diff_density_max 0.32 _refine_ls_number_reflns 2154 _refine_ls_number_restraints 5 _refine_ls_number_parameters 166 _refine_ls_wR_factor_ref 0.0347 _refine_ls_goodness_of_fit_ref 0.9154 _refine_ls_R_factor_all 0.0480 _refine_ls_wR_factor_all 0.0524 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 2154 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_gt 0.0347 _refine_ls_shift/su_max 0.001 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.456 0.201 0.181 ; _refine_ls_extinction_method None _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 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_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ti1 Ti 0.88971(5) 0.2500 0.44489(2) 0.0159 1.0000 Uani S T . . . . Cl1 Cl 0.80012(5) 0.37983(3) 0.50522(2) 0.0234 1.0000 Uani . . . . . . N1 N 1.1069(2) 0.2500 0.51338(10) 0.0197 1.0000 Uani S T . . . . N2 N 1.05349(16) 0.34520(11) 0.39291(7) 0.0179 1.0000 Uani . . . . . . N3 N 0.7593(2) 0.2500 0.38687(11) 0.0190 1.0000 Uani S T . . . . C1 C 1.2205(3) 0.2500 0.46244(13) 0.0201 1.0000 Uani S T . . . . C2 C 1.2003(2) 0.33867(14) 0.42170(9) 0.0202 1.0000 Uani . . . . . . C3 C 1.0538(2) 0.30478(14) 0.32775(8) 0.0201 1.0000 Uani . . . . . . C4 C 1.3760(3) 0.250000(7) 0.48775(14) 0.0257 1.0000 Uani S T . . . . C5 C 1.1182(2) 0.33456(15) 0.55566(10) 0.0261 1.0000 Uani . . . . . . C6 C 1.0213(2) 0.44919(13) 0.38697(10) 0.0238 1.0000 Uani . . . . . . C7 C 0.6418(3) 0.2500 0.34620(12) 0.0185 1.0000 Uani S T . . . . C8 C 0.5813(2) 0.33783(14) 0.32532(9) 0.0209 1.0000 Uani . . . . . . C9 C 0.4692(2) 0.33555(16) 0.28147(10) 0.0255 1.0000 Uani . . . . . . C10 C 0.4141(3) 0.250000(7) 0.25881(14) 0.0278 1.0000 Uani S T . . . . C11 C 0.6352(2) 0.43302(14) 0.34966(10) 0.0241 1.0000 Uani . . . . . . C12 C 0.6875(3) 0.49690(17) 0.29564(12) 0.0362 1.0000 Uani . . . . . . C13 C 0.5235(2) 0.48498(16) 0.38968(12) 0.0344 1.0000 Uani . . . . . . H21 H 1.2163 0.3961 0.4489 0.0243 1.0000 Uiso R . . . . . H22 H 1.2725 0.3378 0.3867 0.0243 1.0000 Uiso R . . . . . H31 H 1.1415 0.3279 0.3054 0.0251 1.0000 Uiso R . . . . . H32 H 0.9668 0.3279 0.3048 0.0251 1.0000 Uiso R . . . . . H41 H 1.4447 0.2500 0.4514 0.0322 1.0000 Uiso RS . . . . . H42 H 1.3918 0.3083 0.5142 0.0322 1.0000 Uiso R . . . . . H51 H 1.0411 0.3317 0.5885 0.0317 1.0000 Uiso R . . . . . H52 H 1.2138 0.3342 0.5769 0.0317 1.0000 Uiso R . . . . . H53 H 1.1075 0.3944 0.5302 0.0317 1.0000 Uiso R . . . . . H61 H 0.9240 0.4579 0.3681 0.0295 1.0000 Uiso R . . . . . H62 H 1.0243 0.4795 0.4299 0.0295 1.0000 Uiso R . . . . . H63 H 1.0944 0.4799 0.3590 0.0295 1.0000 Uiso R . . . . . H91 H 0.4273 0.3972 0.2663 0.0292 1.0000 Uiso R . . . . . H101 H 0.3360 0.2500 0.2264 0.0339 1.0000 Uiso RS . . . . . H111 H 0.7193 0.4200 0.3776 0.0298 1.0000 Uiso R . . . . . H121 H 0.7229 0.5592 0.3127 0.0466 1.0000 Uiso R . . . . . H122 H 0.7667 0.4639 0.2725 0.0466 1.0000 Uiso R . . . . . H123 H 0.6061 0.5088 0.2659 0.0466 1.0000 Uiso R . . . . . H131 H 0.5632 0.5471 0.4051 0.0430 1.0000 Uiso R . . . . . H132 H 0.4965 0.4443 0.4268 0.0430 1.0000 Uiso R . . . . . H133 H 0.4369 0.4973 0.3631 0.0430 1.0000 Uiso R . . . . . C101 C 0.6255(3) 0.250000(10) 0.62529(16) 0.0396 1.0000 Uani S T . . . . Cl101 Cl 0.76382(15) 0.27648(17) 0.67883(7) 0.0714 0.5000 Uani . . . . . . Cl102 Cl 0.45780(9) 0.2500 0.66415(4) 0.0353 1.0000 Uani S T . . . . H1011 H 0.6325 0.3083 0.5981 0.0495 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0154(2) 0.0165(2) 0.0159(2) 0.0000 -0.00010(19) 0.0000 Cl1 0.0243(2) 0.0229(2) 0.0231(2) -0.00451(19) 0.00142(18) 0.00273(19) N1 0.0193(11) 0.0212(11) 0.0186(10) 0.0000 0.0005(9) 0.0000 N2 0.0175(7) 0.0170(7) 0.0191(7) -0.0005(6) -0.0003(6) -0.0007(6) N3 0.0180(10) 0.0188(10) 0.0203(11) 0.0000 0.0007(9) 0.0000 C1 0.0148(12) 0.0234(13) 0.0220(13) 0.0000 0.0022(10) 0.0000 C2 0.0153(8) 0.0240(10) 0.0213(9) 0.0021(8) -0.0009(7) -0.0039(7) C3 0.0213(9) 0.0228(10) 0.0163(8) 0.0018(7) 0.0000(7) -0.0008(8) C4 0.0173(13) 0.0329(15) 0.0271(14) 0.0000 -0.0040(11) 0.0000 C5 0.0233(10) 0.0309(11) 0.0241(9) -0.0080(9) -0.0025(8) -0.0005(9) C6 0.0250(10) 0.0157(9) 0.0307(10) 0.0026(8) 0.0010(8) -0.0006(8) C7 0.0154(12) 0.0217(13) 0.0184(12) 0.0000 0.0011(10) 0.0000 C8 0.0195(9) 0.0230(10) 0.0204(9) 0.0034(8) 0.0014(7) 0.0004(8) C9 0.0197(9) 0.0320(11) 0.0248(9) 0.0044(9) -0.0014(8) 0.0025(8) C10 0.0166(13) 0.0420(18) 0.0246(14) 0.0000 -0.0042(11) 0.0000 C11 0.0216(10) 0.0206(10) 0.0302(10) 0.0067(8) -0.0019(8) -0.0006(8) C12 0.0384(13) 0.0307(12) 0.0396(13) 0.0139(10) -0.0010(10) -0.0058(10) C13 0.0324(11) 0.0266(11) 0.0443(13) -0.0032(10) 0.0035(10) -0.0043(9) C101 0.0245(16) 0.070(2) 0.0242(14) 0.0000 0.0012(13) 0.0000 Cl101 0.0408(6) 0.128(3) 0.0454(6) 0.0068(9) -0.0195(5) -0.0135(9) Cl102 0.0337(4) 0.0436(5) 0.0285(4) 0.0000 0.0059(3) 0.0000 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 . N2 5_555 2.3069(16) yes Ti1 . Cl1 5_555 2.3715(5) yes Ti1 . Cl1 . 2.3715(5) yes Ti1 . N1 . 2.492(2) yes Ti1 . N2 . 2.3069(16) yes Ti1 . N3 . 1.728(2) yes N1 . C5 5_555 1.486(2) yes N1 . C1 . 1.511(3) yes N1 . C5 . 1.486(2) yes N2 . C2 . 1.504(2) yes N2 . C3 . 1.487(2) yes N2 . C6 . 1.491(2) yes N3 . C7 . 1.394(3) yes C1 . C2 5_555 1.521(2) yes C1 . C2 . 1.521(2) yes C1 . C4 . 1.548(4) yes C2 . H21 . 1.000 no C2 . H22 . 1.000 no C3 . C3 5_555 1.533(4) yes C3 . H31 . 1.000 no C3 . H32 . 1.000 no C4 . H42 5_555 1.000 no C4 . H41 . 1.000 no C4 . H42 . 1.000 no C5 . H51 . 1.000 no C5 . H52 . 1.000 no C5 . H53 . 1.000 no C6 . H61 . 1.000 no C6 . H62 . 1.000 no C6 . H63 . 1.000 no C7 . C8 5_555 1.423(2) yes C7 . C8 . 1.423(2) yes C8 . C9 . 1.399(3) yes C8 . C11 . 1.514(3) yes C9 . C10 . 1.388(3) yes C9 . H91 . 1.000 no C10 . H101 . 1.000 no C11 . C12 . 1.529(3) yes C11 . C13 . 1.527(3) yes C11 . H111 . 1.000 no C12 . H121 . 1.000 no C12 . H122 . 1.000 no C12 . H123 . 1.000 no C13 . H131 . 1.000 no C13 . H132 . 1.000 no C13 . H133 . 1.000 no C101 . H1011 5_555 1.000 no C101 . Cl101 5_555 1.757(3) yes C101 . Cl101 . 1.757(3) yes C101 . Cl102 . 1.769(3) yes C101 . H1011 . 1.000 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 N2 5_555 Ti1 . Cl1 5_555 92.70(4) yes N2 5_555 Ti1 . Cl1 . 158.77(4) yes Cl1 5_555 Ti1 . Cl1 . 100.02(3) yes N2 5_555 Ti1 . N1 . 74.66(6) yes Cl1 5_555 Ti1 . N1 . 88.63(4) yes Cl1 . Ti1 . N1 . 88.63(4) yes N2 5_555 Ti1 . N2 . 70.56(8) yes Cl1 5_555 Ti1 . N2 . 158.77(4) yes Cl1 . Ti1 . N2 . 92.70(4) yes N1 . Ti1 . N2 . 74.66(6) yes N2 5_555 Ti1 . N3 . 97.53(7) yes Cl1 5_555 Ti1 . N3 . 97.56(5) yes Cl1 . Ti1 . N3 . 97.56(5) yes N1 . Ti1 . N3 . 170.32(9) yes N2 . Ti1 . N3 . 97.53(7) yes C5 5_555 N1 . Ti1 . 113.97(12) yes C5 5_555 N1 . C1 . 112.16(14) yes Ti1 . N1 . C1 . 99.20(15) yes C5 5_555 N1 . C5 . 105.6(2) yes Ti1 . N1 . C5 . 113.97(12) yes C1 . N1 . C5 . 112.16(14) yes Ti1 . N2 . C2 . 112.23(11) yes Ti1 . N2 . C3 . 102.79(11) yes C2 . N2 . C3 . 110.41(15) yes Ti1 . N2 . C6 . 118.02(12) yes C2 . N2 . C6 . 106.11(14) yes C3 . N2 . C6 . 107.10(14) yes Ti1 . N3 . C7 . 172.9(2) yes C2 5_555 C1 . N1 . 108.34(14) yes C2 5_555 C1 . C2 . 109.3(2) yes N1 . C1 . C2 . 108.34(14) yes C2 5_555 C1 . C4 . 108.15(15) yes N1 . C1 . C4 . 114.5(2) yes C2 . C1 . C4 . 108.15(15) yes C1 . C2 . N2 . 113.04(17) yes C1 . C2 . H21 . 108.2 no N2 . C2 . H21 . 108.6 no C1 . C2 . H22 . 108.9 no N2 . C2 . H22 . 108.5 no H21 . C2 . H22 . 109.5 no C3 5_555 C3 . N2 . 112.36(9) yes C3 5_555 C3 . H31 . 108.9 no N2 . C3 . H31 . 108.4 no C3 5_555 C3 . H32 . 108.9 no N2 . C3 . H32 . 108.8 no H31 . C3 . H32 . 109.5 no C1 . C4 . H42 5_555 109.3 no C1 . C4 . H41 . 109.8 no H42 5_555 C4 . H41 . 109.5 no C1 . C4 . H42 . 109.3 no H42 5_555 C4 . H42 . 109.5 no H41 . C4 . H42 . 109.5 no N1 . C5 . H51 . 109.5 no N1 . C5 . H52 . 109.2 no H51 . C5 . H52 . 109.5 no N1 . C5 . H53 . 109.7 no H51 . C5 . H53 . 109.5 no H52 . C5 . H53 . 109.5 no N2 . C6 . H61 . 109.6 no N2 . C6 . H62 . 109.4 no H61 . C6 . H62 . 109.5 no N2 . C6 . H63 . 109.4 no H61 . C6 . H63 . 109.5 no H62 . C6 . H63 . 109.5 no C8 5_555 C7 . N3 . 120.25(12) yes C8 5_555 C7 . C8 . 119.5(2) yes N3 . C7 . C8 . 120.25(12) yes C7 . C8 . C9 . 118.87(19) yes C7 . C8 . C11 . 121.53(17) yes C9 . C8 . C11 . 119.60(17) yes C8 . C9 . C10 . 121.7(2) yes C8 . C9 . H91 . 119.0 no C10 . C9 . H91 . 119.3 no C9 . C10 . C9 5_555 119.2(3) yes C9 . C10 . H101 . 120.4 no C9 5_555 C10 . H101 . 120.4 no C8 . C11 . C12 . 111.58(18) yes C8 . C11 . C13 . 112.28(17) yes C12 . C11 . C13 . 110.64(18) yes C8 . C11 . H111 . 107.5 no C12 . C11 . H111 . 107.2 no C13 . C11 . H111 . 107.3 no C11 . C12 . H121 . 110.3 no C11 . C12 . H122 . 109.3 no H121 . C12 . H122 . 109.5 no C11 . C12 . H123 . 108.8 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no C11 . C13 . H131 . 109.9 no C11 . C13 . H132 . 109.5 no H131 . C13 . H132 . 109.5 no C11 . C13 . H133 . 109.0 no H131 . C13 . H133 . 109.5 no H132 . C13 . H133 . 109.5 no H1011 5_555 C101 . Cl101 5_555 98.5 no H1011 5_555 C101 . Cl101 . 119.5 no Cl101 5_555 C101 . Cl101 . 24.36(16) yes H1011 5_555 C101 . Cl102 . 108.9 no Cl101 5_555 C101 . Cl102 . 110.73(18) yes Cl101 . C101 . Cl102 . 110.73(18) yes H1011 5_555 C101 . H1011 . 109.5 no Cl101 5_555 C101 . H1011 . 119.5 no Cl101 . C101 . H1011 . 98.5 no Cl102 . C101 . H1011 . 108.9 no #===end data_COMPOUND_4-trans _database_code_depnum_ccdc_archive 'CCDC 676930' # Local code CW11 _chemical_name_systematic ; Ti(N-2-C6H4tBu)(Me4DACH)Cl2 ; _publ_section_exptl_refinement ; The Flack parameter of 0.56(5) (2167 Friedel pairs) indicates that CW11 is probably an intimate twin ; _chemical_melting_point ? _cell_length_a 23.3237(9) _cell_length_b 12.9435(4) _cell_length_c 7.7526(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2340.43(15) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n a 21 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x+1/2,y+1/2,z+1/2 x+1/2,-y+1/2,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 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' Ti 0.2776 0.4457 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C20 H36 Cl2 N4 Ti1' _chemical_formula_moiety 'C20 H36 Cl2 N4 Ti1' _chemical_compound_source ? _chemical_formula_weight 451.34 _cell_measurement_reflns_used 2903 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_min 0.11 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_max 0.15 _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_meas ? _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 0.606 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 0.94 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 5186 _reflns_number_total 4998 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_min 5.245 _diffrn_reflns_theta_max 27.445 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.347 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _reflns_limit_h_min 0 _reflns_limit_h_max 30 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min -9 _reflns_limit_l_max 9 _oxford_diffrn_Wilson_B_factor 2.34 _oxford_diffrn_Wilson_scale 15.77 _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.29 _refine_diff_density_max 0.49 _refine_ls_number_reflns 2767 _refine_ls_number_restraints 1 _refine_ls_number_parameters 245 _refine_ls_wR_factor_ref 0.0478 _refine_ls_goodness_of_fit_ref 1.0876 _refine_ls_R_factor_all 0.1212 _refine_ls_wR_factor_all 0.1013 _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 2767 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_gt 0.0478 _refine_ls_shift/su_max 0.000341 _refine_ls_abs_structure_Flack 0.56(5) _refine_ls_abs_structure_details 'Flack (1983), 2167 Friedel-pairs' _chemical_absolute_configuration ad _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.994 0.259E-01 0.764 ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. 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_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ti1 Ti 0.31536(3) 0.78019(6) 0.93251(17) 0.0257 1.0000 Uani . . . . . . N1 N 0.22103(17) 0.7788(3) 1.0809(5) 0.0307 1.0000 Uani . . . . . . N2 N 0.32623(16) 0.8837(3) 1.1639(5) 0.0291 1.0000 Uani . . . . . . N3 N 0.33396(18) 0.6808(3) 1.1724(6) 0.0350 1.0000 Uani . . . . . . N4 N 0.38296(17) 0.8011(3) 0.8490(5) 0.0298 1.0000 Uani . . . . . . C1 C 0.2432(2) 0.7738(3) 1.2620(7) 0.0327 1.0000 Uani . . . . . . C2 C 0.2794(2) 0.8704(4) 1.2956(6) 0.0340 1.0000 Uani . . . . . . C3 C 0.3815(2) 0.8492(4) 1.2398(8) 0.0412 1.0000 Uani . . . . . . C4 C 0.3806(2) 0.7329(4) 1.2719(8) 0.0405 1.0000 Uani . . . . . . C5 C 0.2810(2) 0.6778(4) 1.2792(7) 0.0386 1.0000 Uani . . . . . . C6 C 0.1963(2) 0.7667(4) 1.4005(7) 0.0412 1.0000 Uani . . . . . . C7 C 0.1852(2) 0.6884(4) 1.0307(7) 0.0431 1.0000 Uani . . . . . . C8 C 0.1837(2) 0.8699(4) 1.0530(7) 0.0424 1.0000 Uani . . . . . . C9 C 0.3325(2) 0.9949(4) 1.1209(7) 0.0385 1.0000 Uani . . . . . . C10 C 0.3531(3) 0.5721(4) 1.1413(8) 0.0488 1.0000 Uani . . . . . . C11 C 0.4240(2) 0.8482(4) 0.7431(7) 0.0365 1.0000 Uani . . . . . . C12 C 0.4754(2) 0.7999(5) 0.6874(7) 0.0454 1.0000 Uani . . . . . . C13 C 0.5107(2) 0.8586(6) 0.5764(9) 0.0566 1.0000 Uani . . . . . . C14 C 0.4976(3) 0.9585(6) 0.5260(8) 0.0614 1.0000 Uani . . . . . . C15 C 0.4480(3) 1.0039(5) 0.5794(8) 0.0490 1.0000 Uani . . . . . . C16 C 0.4117(2) 0.9494(4) 0.6866(7) 0.0392 1.0000 Uani . . . . . . C17 C 0.4929(2) 0.6921(5) 0.7469(9) 0.0533 1.0000 Uani . . . . . . C18 C 0.5507(3) 0.6562(7) 0.6692(12) 0.0869 1.0000 Uani . . . . . . C19 C 0.5004(3) 0.6922(5) 0.9433(11) 0.0624 1.0000 Uani . . . . . . C20 C 0.4482(3) 0.6112(5) 0.6925(9) 0.0601 1.0000 Uani . . . . . . Cl1 Cl 0.28986(6) 0.63257(9) 0.7717(2) 0.0403 1.0000 Uani . . . . . . Cl2 Cl 0.27015(5) 0.90411(9) 0.7536(2) 0.0373 1.0000 Uani . . . . . . H21 H 0.2970 0.8650 1.4128 0.0410 1.0000 Uiso R . . . . . H22 H 0.2539 0.9324 1.2909 0.0410 1.0000 Uiso R . . . . . H31 H 0.3871 0.8856 1.3523 0.0509 1.0000 Uiso R . . . . . H32 H 0.4135 0.8674 1.1597 0.0509 1.0000 Uiso R . . . . . H41 H 0.3748 0.7191 1.3976 0.0506 1.0000 Uiso R . . . . . H42 H 0.4183 0.7035 1.2346 0.0506 1.0000 Uiso R . . . . . H51 H 0.2927 0.6710 1.4027 0.0492 1.0000 Uiso R . . . . . H52 H 0.2580 0.6159 1.2445 0.0492 1.0000 Uiso R . . . . . H61 H 0.2146 0.7636 1.5170 0.0525 1.0000 Uiso R . . . . . H62 H 0.1709 0.8289 1.3937 0.0525 1.0000 Uiso R . . . . . H63 H 0.1729 0.7030 1.3815 0.0525 1.0000 Uiso R . . . . . H71 H 0.1716 0.6967 0.9091 0.0564 1.0000 Uiso R . . . . . H72 H 0.1513 0.6833 1.1094 0.0564 1.0000 Uiso R . . . . . H73 H 0.2088 0.6242 1.0404 0.0564 1.0000 Uiso R . . . . . H81 H 0.1698 0.8703 0.9310 0.0542 1.0000 Uiso R . . . . . H82 H 0.2060 0.9344 1.0760 0.0542 1.0000 Uiso R . . . . . H83 H 0.1501 0.8665 1.1331 0.0542 1.0000 Uiso R . . . . . H91 H 0.3635 1.0040 1.0330 0.0491 1.0000 Uiso R . . . . . H92 H 0.3425 1.0347 1.2273 0.0491 1.0000 Uiso R . . . . . H93 H 0.2954 1.0209 1.0731 0.0491 1.0000 Uiso R . . . . . H101 H 0.3228 0.5349 1.0744 0.0580 1.0000 Uiso R . . . . . H102 H 0.3592 0.5366 1.2543 0.0580 1.0000 Uiso R . . . . . H103 H 0.3897 0.5721 1.0743 0.0580 1.0000 Uiso R . . . . . H131 H 0.5461 0.8254 0.5292 0.0740 1.0000 Uiso R . . . . . H141 H 0.5250 0.9979 0.4518 0.0710 1.0000 Uiso R . . . . . H151 H 0.4381 1.0754 0.5403 0.0577 1.0000 Uiso R . . . . . H161 H 0.3757 0.9830 0.7281 0.0517 1.0000 Uiso R . . . . . H181 H 0.5610 0.5856 0.7112 0.1185 1.0000 Uiso R . . . . . H182 H 0.5816 0.7060 0.7022 0.1185 1.0000 Uiso R . . . . . H183 H 0.5466 0.6550 0.5408 0.1185 1.0000 Uiso R . . . . . H191 H 0.5114 0.6210 0.9806 0.0754 1.0000 Uiso R . . . . . H192 H 0.5313 0.7419 0.9768 0.0754 1.0000 Uiso R . . . . . H193 H 0.4637 0.7124 1.0004 0.0754 1.0000 Uiso R . . . . . H201 H 0.4603 0.5415 0.7346 0.0724 1.0000 Uiso R . . . . . H202 H 0.4099 0.6289 0.7422 0.0724 1.0000 Uiso R . . . . . H203 H 0.4456 0.6103 0.5637 0.0724 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0307(4) 0.0238(4) 0.0226(4) -0.0005(5) 0.0004(4) 0.0000(4) N1 0.030(2) 0.029(2) 0.033(2) -0.002(2) 0.0008(17) 0.0000(19) N2 0.027(2) 0.030(2) 0.030(2) -0.0035(18) 0.0013(17) -0.0059(17) N3 0.037(2) 0.031(2) 0.037(2) 0.003(2) -0.005(2) 0.0006(18) N4 0.031(2) 0.029(2) 0.029(2) 0.0034(17) -0.0001(18) -0.0029(15) C1 0.041(3) 0.031(2) 0.025(2) 0.000(3) 0.001(2) -0.005(2) C2 0.039(3) 0.034(2) 0.029(3) 0.002(2) 0.007(2) -0.007(2) C3 0.026(3) 0.056(3) 0.041(3) -0.005(3) -0.004(3) -0.007(2) C4 0.034(3) 0.052(3) 0.036(3) 0.007(3) -0.010(3) 0.002(2) C5 0.041(3) 0.041(3) 0.033(3) 0.007(3) 0.001(3) -0.004(2) C6 0.043(3) 0.044(3) 0.036(4) -0.001(2) 0.012(2) -0.005(2) C7 0.034(3) 0.052(3) 0.044(3) -0.008(3) 0.001(3) -0.008(3) C8 0.040(3) 0.045(3) 0.043(3) 0.006(3) -0.005(3) 0.008(3) C9 0.043(3) 0.026(3) 0.046(3) 0.000(2) 0.013(2) -0.009(2) C10 0.061(4) 0.032(3) 0.054(4) 0.012(3) 0.012(3) 0.008(3) C11 0.039(3) 0.040(3) 0.030(3) -0.002(3) -0.008(3) -0.002(2) C12 0.034(3) 0.065(4) 0.038(3) -0.005(3) 0.008(2) -0.004(3) C13 0.033(3) 0.077(5) 0.060(4) -0.005(4) 0.010(3) -0.002(3) C14 0.054(4) 0.085(6) 0.046(4) 0.005(4) 0.004(3) -0.030(4) C15 0.053(4) 0.054(4) 0.041(3) 0.000(3) -0.003(3) -0.014(3) C16 0.040(3) 0.040(3) 0.037(3) -0.002(2) -0.004(2) -0.005(2) C17 0.032(3) 0.068(4) 0.060(4) -0.016(3) 0.002(3) 0.014(3) C18 0.045(4) 0.103(6) 0.113(7) -0.008(5) 0.008(4) 0.030(4) C19 0.053(4) 0.063(4) 0.071(5) 0.006(4) -0.013(4) 0.010(3) C20 0.056(4) 0.054(4) 0.071(5) -0.003(3) -0.007(3) 0.024(3) Cl1 0.0491(7) 0.0331(6) 0.0387(7) -0.0095(7) -0.0011(7) -0.0073(5) Cl2 0.0440(6) 0.0366(6) 0.0314(6) 0.0048(6) 0.0009(7) 0.0069(5) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2643(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 Ti1 . N1 . 2.483(4) yes Ti1 . N2 . 2.253(4) yes Ti1 . N3 . 2.302(4) yes Ti1 . N4 . 1.726(4) yes Ti1 . Cl1 . 2.3577(14) yes Ti1 . Cl2 . 2.3683(14) yes N1 . C1 . 1.498(7) yes N1 . C7 . 1.490(6) yes N1 . C8 . 1.482(6) yes N2 . C2 . 1.505(6) yes N2 . C3 . 1.486(6) yes N2 . C9 . 1.485(6) yes N3 . C4 . 1.495(7) yes N3 . C5 . 1.488(7) yes N3 . C10 . 1.495(6) yes N4 . C11 . 1.401(7) yes C1 . C2 . 1.531(6) yes C1 . C5 . 1.529(7) yes C1 . C6 . 1.536(7) yes C2 . H21 . 1.000 no C2 . H22 . 1.000 no C3 . C4 . 1.525(8) yes C3 . H31 . 1.000 no C3 . H32 . 1.000 no C4 . H41 . 1.000 no C4 . H42 . 1.000 no C5 . H51 . 1.000 no C5 . H52 . 1.000 no C6 . H61 . 1.000 no C6 . H62 . 1.000 no C6 . H63 . 1.000 no C7 . H71 . 1.000 no C7 . H72 . 1.000 no C7 . H73 . 1.000 no C8 . H81 . 1.000 no C8 . H82 . 1.000 no C8 . H83 . 1.000 no C9 . H91 . 1.000 no C9 . H92 . 1.000 no C9 . H93 . 1.000 no C10 . H101 . 1.000 no C10 . H102 . 1.000 no C10 . H103 . 1.000 no C11 . C12 . 1.419(7) yes C11 . C16 . 1.411(7) yes C12 . C13 . 1.413(9) yes C12 . C17 . 1.525(9) yes C13 . C14 . 1.385(10) yes C13 . H131 . 1.000 no C14 . C15 . 1.364(9) yes C14 . H141 . 1.000 no C15 . C16 . 1.380(8) yes C15 . H151 . 1.000 no C16 . H161 . 1.000 no C17 . C18 . 1.548(8) yes C17 . C19 . 1.533(10) yes C17 . C20 . 1.537(9) yes C18 . H181 . 1.000 no C18 . H182 . 1.000 no C18 . H183 . 1.000 no C19 . H191 . 1.000 no C19 . H192 . 1.000 no C19 . H193 . 1.000 no C20 . H201 . 1.000 no C20 . H202 . 1.000 no C20 . H203 . 1.000 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 N1 . Ti1 . N2 . 74.64(14) yes N1 . Ti1 . N3 . 77.80(14) yes N2 . Ti1 . N3 . 70.61(15) yes N1 . Ti1 . N4 . 169.93(17) yes N2 . Ti1 . N4 . 95.91(17) yes N3 . Ti1 . N4 . 102.62(18) yes N1 . Ti1 . Cl1 . 90.90(10) yes N2 . Ti1 . Cl1 . 158.62(11) yes N3 . Ti1 . Cl1 . 91.25(12) yes N4 . Ti1 . Cl1 . 99.14(14) yes N1 . Ti1 . Cl2 . 83.21(10) yes N2 . Ti1 . Cl2 . 96.53(11) yes N3 . Ti1 . Cl2 . 159.29(12) yes N4 . Ti1 . Cl2 . 94.63(14) yes Cl1 . Ti1 . Cl2 . 97.29(6) yes Ti1 . N1 . C1 . 97.4(3) yes Ti1 . N1 . C7 . 112.5(3) yes C1 . N1 . C7 . 113.9(4) yes Ti1 . N1 . C8 . 116.6(3) yes C1 . N1 . C8 . 112.0(4) yes C7 . N1 . C8 . 104.9(4) yes Ti1 . N2 . C2 . 113.0(3) yes Ti1 . N2 . C3 . 103.5(3) yes C2 . N2 . C3 . 109.1(4) yes Ti1 . N2 . C9 . 114.1(3) yes C2 . N2 . C9 . 109.6(4) yes C3 . N2 . C9 . 107.1(4) yes Ti1 . N3 . C4 . 107.6(3) yes Ti1 . N3 . C5 . 107.9(3) yes C4 . N3 . C5 . 109.2(4) yes Ti1 . N3 . C10 . 116.9(3) yes C4 . N3 . C10 . 106.9(4) yes C5 . N3 . C10 . 108.2(4) yes Ti1 . N4 . C11 . 155.9(4) yes N1 . C1 . C2 . 108.3(4) yes N1 . C1 . C5 . 108.4(4) yes C2 . C1 . C5 . 109.3(4) yes N1 . C1 . C6 . 114.3(4) yes C2 . C1 . C6 . 108.8(4) yes C5 . C1 . C6 . 107.6(4) yes C1 . C2 . N2 . 112.3(4) yes C1 . C2 . H21 . 109.0 no N2 . C2 . H21 . 109.0 no C1 . C2 . H22 . 108.8 no N2 . C2 . H22 . 108.3 no H21 . C2 . H22 . 109.5 no N2 . C3 . C4 . 110.5(4) yes N2 . C3 . H31 . 108.5 no C4 . C3 . H31 . 108.9 no N2 . C3 . H32 . 109.4 no C4 . C3 . H32 . 110.1 no H31 . C3 . H32 . 109.5 no C3 . C4 . N3 . 111.7(4) yes C3 . C4 . H41 . 109.7 no N3 . C4 . H41 . 108.9 no C3 . C4 . H42 . 108.5 no N3 . C4 . H42 . 108.5 no H41 . C4 . H42 . 109.5 no C1 . C5 . N3 . 114.1(4) yes C1 . C5 . H51 . 108.3 no N3 . C5 . H51 . 107.9 no C1 . C5 . H52 . 108.6 no N3 . C5 . H52 . 108.4 no H51 . C5 . H52 . 109.5 no C1 . C6 . H61 . 109.2 no C1 . C6 . H62 . 109.7 no H61 . C6 . H62 . 109.5 no C1 . C6 . H63 . 109.5 no H61 . C6 . H63 . 109.5 no H62 . C6 . H63 . 109.5 no N1 . C7 . H71 . 109.8 no N1 . C7 . H72 . 109.7 no H71 . C7 . H72 . 109.5 no N1 . C7 . H73 . 108.9 no H71 . C7 . H73 . 109.5 no H72 . C7 . H73 . 109.5 no N1 . C8 . H81 . 109.5 no N1 . C8 . H82 . 109.4 no H81 . C8 . H82 . 109.5 no N1 . C8 . H83 . 109.6 no H81 . C8 . H83 . 109.5 no H82 . C8 . H83 . 109.5 no N2 . C9 . H91 . 109.8 no N2 . C9 . H92 . 109.7 no H91 . C9 . H92 . 109.5 no N2 . C9 . H93 . 108.9 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no N3 . C10 . H101 . 109.1 no N3 . C10 . H102 . 109.5 no H101 . C10 . H102 . 109.5 no N3 . C10 . H103 . 109.8 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no N4 . C11 . C12 . 124.3(5) yes N4 . C11 . C16 . 116.6(5) yes C12 . C11 . C16 . 119.1(5) yes C11 . C12 . C13 . 116.2(6) yes C11 . C12 . C17 . 122.5(5) yes C13 . C12 . C17 . 121.3(5) yes C12 . C13 . C14 . 123.0(6) yes C12 . C13 . H131 . 118.3 no C14 . C13 . H131 . 118.7 no C13 . C14 . C15 . 120.3(6) yes C13 . C14 . H141 . 119.9 no C15 . C14 . H141 . 119.8 no C14 . C15 . C16 . 118.8(6) yes C14 . C15 . H151 . 120.2 no C16 . C15 . H151 . 120.9 no C11 . C16 . C15 . 122.5(5) yes C11 . C16 . H161 . 118.3 no C15 . C16 . H161 . 119.1 no C12 . C17 . C18 . 113.0(6) yes C12 . C17 . C19 . 109.3(5) yes C18 . C17 . C19 . 106.7(6) yes C12 . C17 . C20 . 111.0(5) yes C18 . C17 . C20 . 106.2(6) yes C19 . C17 . C20 . 110.5(6) yes C17 . C18 . H181 . 110.9 no C17 . C18 . H182 . 109.6 no H181 . C18 . H182 . 109.5 no C17 . C18 . H183 . 107.9 no H181 . C18 . H183 . 109.5 no H182 . C18 . H183 . 109.5 no C17 . C19 . H191 . 108.5 no C17 . C19 . H192 . 109.9 no H191 . C19 . H192 . 109.5 no C17 . C19 . H193 . 110.0 no H191 . C19 . H193 . 109.5 no H192 . C19 . H193 . 109.5 no C17 . C20 . H201 . 109.4 no C17 . C20 . H202 . 110.1 no H201 . C20 . H202 . 109.5 no C17 . C20 . H203 . 108.8 no H201 . C20 . H203 . 109.5 no H202 . C20 . H203 . 109.5 no #===end