# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2004
data_global
#===================================================================
_journal_coden_Cambridge 182
loop_
_publ_author_name
'Matthias Tamm'
'Thomas Bannenberg'
'Eberhardt Herdtweck'
'Soren Randoll'
_publ_contact_author_name 'Prof Matthias Tamm'
_publ_contact_author_address
;
Anorganisch-Chemisches
Technische Universitat Munchen
Garching
GERMANY
;
_publ_contact_author_email MATTHIAS.TAMM@CH.TUM.DE
_publ_requested_journal 'Chemical Communications'
_publ_section_title
;
Titanium Complexes with Imidazolin-2-iminato
Ligands
;
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C.,
Polidori, G. & Camalli, M. (1994). SIR92, J. Appl. Cryst. 27, 435-436.
Nonius (2001a). Data Collection Software for Nonius Kappa-CCD devices.
Nonius BV, Delft, The Netherlands.
Nonius (2001b). DENZO Processing Software for Nonius Kappa-CCD devices,
Nonius BV, Delft, The Netherlands.
Sheldrick, G. M. (1998). SHELXL97, University of Gottingen, Gottingen,
Germany.
Spek, A. L. (2001). PLATON, A Multipurpose Crystallographic Tool, Utrecht
University, Utrecht, The Netherlands.
;
#===================================================================
data_RANE-4317-173
_database_code_depnum_ccdc_archive 'CCDC 229688'
#===================================================================
# 0. AUDIT DETAILS
_audit_creation_date 24-Oct-03
_audit_creation_method 'PLATON
option'
_audit_update_record
;
24-Oct-03 Updated by the Author E.H.
Textwriting by E.H.
Checkcif OK
14-Jan-04 Updated by the Author E.H.
20-Jan-04 Updated by the Author E.H.
;
#===================================================================
# 5. CHEMICAL DATA
#===================================================================
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_formula_moiety 'C14 H29 N3 Si'
_chemical_formula_structural ?
_chemical_formula_analytical ?
_chemical_formula_sum 'C14 H29 N3 Si'
_chemical_formula_weight 267.49
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#===================================================================
# 6. CRYSTAL DATA
#===================================================================
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
_cell_length_a 9.0758(2)
_cell_length_b 9.4187(2)
_cell_length_c 11.0961(3)
_cell_angle_alpha 84.7122(12)
_cell_angle_beta 83.0332(13)
_cell_angle_gamma 63.7546(9)
_cell_volume 843.66(4)
_cell_formula_units_Z 2
_cell_measurement_temperature 173(1)
_cell_measurement_reflns_used 3090
_cell_measurement_theta_min 1.85
_cell_measurement_theta_max 25.40
_exptl_crystal_description fragment
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.53
_exptl_crystal_size_mid 0.46
_exptl_crystal_size_min 0.35
_exptl_crystal_density_meas none
_exptl_crystal_density_diffrn 1.053
_exptl_crystal_density_method none
_exptl_crystal_F_000 296
_exptl_absorpt_coefficient_mu 0.130
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.955
_exptl_absorpt_correction_T_max 0.965
_exptl_absorpt_process_details
'(applied during the scaling procedure; Nonius, 2001b)'
_exptl_special_details
;
Diffractometer operator E. Herdtweck
scanspeed 2 x 25 s per film
repetition 1
dx 40
516 films measured in 9 data sets
set 1: phi-scan with delta_phi = 2.0
set 2 to 9 omega-scans with delta_omega = 2.0
;
_publ_section_exptl_prep
;
The crystal was fixed in a capillary with perfluorinated ether and
transferred to the diffractometer.
;
_publ_section_exptl_refinement
;
Straight forward after integration with the program NPROCESS,
source: Nonius (2001b).
Hydrogen atoms could be located in the difference Fourier maps
and refined freely.
;
#===================================================================
# 7. EXPERIMENTAL DATA
#===================================================================
_diffrn_ambient_temperature 173(1)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_source 'NONIUS FR 591 rotating anode'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device ' \k-geometry diffractometer '
_diffrn_measurement_device_type ' Nonius \k-CCD diffractometer'
_diffrn_measurement_method ' phi- and omega-rotation '
_diffrn_detector ' CCD plate '
_diffrn_detector_area_resol_mean 18 # 9 for binned mode
_diffrn_standards_decay_% 0
# number of measured reflections (redundant set)
_diffrn_reflns_number 18531
_diffrn_reflns_av_R_equivalents 0.042
_diffrn_reflns_av_sigmaI/netI 0.0257
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_theta_min 1.85
_diffrn_reflns_theta_max 25.40
_reflns_number_total 3097
_reflns_number_gt 2758
# number of observed reflections (> n sig(I))
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'Kappa-CCD Control Software (Nonius, 2001a)'
_computing_cell_refinement 'DENZO (Nonius, 2001b)'
_computing_data_reduction 'DENZO (Nonius, 2001b)'
_computing_structure_solution 'SIR92 (Altomare, 1994)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)'
_computing_molecular_graphics 'PLATON (Spek, 2001)'
_computing_publication_material 'PLATON (Spek, 2001)'
#===================================================================
# 8. REFINEMENT DATA
#===================================================================
_refine_special_details
;
Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^
or flagged by the user for potential systematic errors. Weighted R-factors
wR and all goodnesses of fit S are based on F^2^, conventional R-factors R
are based on F, with F set to zero for negative F^2^. The observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme sigma
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(Fo^2^)+(0.0549P)^2^+0.5892P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_ls_hydrogen_treatment refall
_refine_ls_number_reflns 3097
_refine_ls_number_parameters 279
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0524
_refine_ls_R_factor_gt 0.0465
_refine_ls_wR_factor_ref 0.1367
_refine_ls_wR_factor_gt 0.1333
_refine_ls_goodness_of_fit_ref 1.149
_refine_ls_restrained_S_all 1.149
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full 25.40
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max 0.481
_refine_diff_density_min -0.241
_refine_diff_density_rms 0.048
#===================================================================
# 9. ATOMIC COORDINATES AND THERMAL PARAMETERS
#===================================================================
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
Si Si Uani 0.12347(7) 0.84057(7) 0.25932(6) 1.000 0.0344(2) . .
N1 N Uani 0.3060(2) 0.6861(2) 0.26453(17) 1.000 0.0341(5) . .
N2 N Uani 0.4735(2) 0.4093(2) 0.30412(16) 1.000 0.0308(5) . .
N3 N Uani 0.5867(2) 0.5414(2) 0.18475(15) 1.000 0.0307(5) . .
C1 C Uani 0.4396(3) 0.5593(2) 0.25118(18) 1.000 0.0290(6) . .
C2 C Uani 0.6367(3) 0.3071(3) 0.2718(2) 1.000 0.0378(7) . .
C3 C Uani 0.7050(3) 0.3865(3) 0.2000(2) 1.000 0.0376(7) . .
C4 C Uani 0.3536(3) 0.3675(3) 0.38516(19) 1.000 0.0342(7) . .
C5 C Uani 0.4370(4) 0.1922(3) 0.4246(3) 1.000 0.0506(9) . .
C6 C Uani 0.2067(3) 0.3973(3) 0.3156(2) 1.000 0.0412(8) . .
C7 C Uani 0.3005(3) 0.4656(3) 0.4987(2) 1.000 0.0418(8) . .
C8 C Uani 0.6141(3) 0.6707(3) 0.11252(19) 1.000 0.0348(7) . .
C9 C Uani 0.4925(3) 0.7392(3) 0.0152(2) 1.000 0.0442(8) . .
C10 C Uani 0.5959(3) 0.7962(3) 0.1986(2) 1.000 0.0420(8) . .
C11 C Uani 0.7889(3) 0.6015(4) 0.0491(3) 1.000 0.0478(9) . .
C12 C Uani 0.0214(4) 0.8369(4) 0.1237(3) 1.000 0.0546(10) . .
C13 C Uani 0.1384(4) 1.0337(3) 0.2517(3) 1.000 0.0531(9) . .
C14 C Uani -0.0233(4) 0.8463(4) 0.3959(3) 1.000 0.0580(10) . .
H21 H Uiso 0.685(3) 0.197(4) 0.296(2) 1.000 0.053(7) . .
H31 H Uiso 0.814(4) 0.351(3) 0.164(3) 1.000 0.056(8) . .
H51 H Uiso 0.475(4) 0.127(4) 0.353(3) 1.000 0.058(8) . .
H52 H Uiso 0.357(3) 0.164(3) 0.476(2) 1.000 0.044(7) . .
H53 H Uiso 0.530(4) 0.174(4) 0.474(3) 1.000 0.063(9) . .
H61 H Uiso 0.240(3) 0.335(4) 0.246(3) 1.000 0.057(8) . .
H62 H Uiso 0.152(3) 0.508(3) 0.285(2) 1.000 0.045(7) . .
H63 H Uiso 0.127(3) 0.370(3) 0.369(2) 1.000 0.050(7) . .
H71 H Uiso 0.256(3) 0.579(4) 0.477(2) 1.000 0.049(7) . .
H72 H Uiso 0.391(4) 0.438(3) 0.546(3) 1.000 0.053(8) . .
H73 H Uiso 0.215(3) 0.443(3) 0.549(2) 1.000 0.043(7) . .
H91 H Uiso 0.379(4) 0.783(3) 0.046(2) 1.000 0.046(7) . .
H92 H Uiso 0.504(4) 0.652(4) -0.042(3) 1.000 0.067(9) . .
H93 H Uiso 0.511(3) 0.821(3) -0.035(3) 1.000 0.057(8) . .
H101 H Uiso 0.683(4) 0.752(3) 0.254(3) 1.000 0.053(8) . .
H102 H Uiso 0.483(4) 0.841(3) 0.246(3) 1.000 0.053(8) . .
H103 H Uiso 0.610(3) 0.880(4) 0.151(3) 1.000 0.058(8) . .
H111 H Uiso 0.869(4) 0.556(3) 0.109(3) 1.000 0.052(8) . .
H112 H Uiso 0.804(4) 0.686(4) -0.002(3) 1.000 0.059(8) . .
H113 H Uiso 0.800(3) 0.517(4) -0.010(3) 1.000 0.058(8) . .
H121 H Uiso -0.002(4) 0.747(4) 0.131(3) 1.000 0.073(10) . .
H122 H Uiso 0.078(4) 0.846(4) 0.046(3) 1.000 0.077(10) . .
H123 H Uiso -0.086(5) 0.927(5) 0.121(3) 1.000 0.088(11) . .
H131 H Uiso 0.208(5) 1.025(5) 0.168(4) 1.000 0.098(12) . .
H132 H Uiso 0.204(4) 1.033(4) 0.321(3) 1.000 0.065(9) . .
H133 H Uiso 0.032(4) 1.122(4) 0.258(3) 1.000 0.070(9) . .
H141 H Uiso -0.042(3) 0.741(4) 0.396(2) 1.000 0.054(8) . .
H142 H Uiso -0.127(5) 0.952(5) 0.400(3) 1.000 0.086(11) . .
H143 H Uiso 0.027(4) 0.847(4) 0.474(3) 1.000 0.086(11) . .
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
Si 0.0291(3) 0.0261(3) 0.0446(4) 0.0002(2) -0.0018(2) -0.0097(3)
N1 0.0305(9) 0.0274(9) 0.0403(10) 0.0004(7) 0.0000(8) -0.0101(8)
N2 0.0312(9) 0.0261(9) 0.0329(9) 0.0001(7) -0.0030(7) -0.0108(7)
N3 0.0279(9) 0.0308(9) 0.0321(9) -0.0016(7) -0.0017(7) -0.0117(7)
C1 0.0317(10) 0.0308(10) 0.0269(10) -0.0014(8) -0.0046(8) -0.0154(9)
C2 0.0329(12) 0.0278(11) 0.0429(12) 0.0003(9) -0.0062(9) -0.0041(9)
C3 0.0278(11) 0.0348(12) 0.0421(12) -0.0032(9) -0.0026(9) -0.0061(9)
C4 0.0408(12) 0.0308(11) 0.0331(11) 0.0026(9) -0.0026(9) -0.0184(10)
C5 0.0568(17) 0.0351(13) 0.0562(16) 0.0104(12) -0.0020(14) -0.0199(12)
C6 0.0452(14) 0.0417(14) 0.0440(13) 0.0005(11) -0.0040(11) -0.0261(12)
C7 0.0496(14) 0.0473(15) 0.0325(12) 0.0010(10) -0.0009(11) -0.0260(12)
C8 0.0356(11) 0.0404(12) 0.0328(11) 0.0011(9) -0.0013(9) -0.0216(10)
C9 0.0456(15) 0.0563(16) 0.0354(12) 0.0098(11) -0.0063(11) -0.0279(13)
C10 0.0467(14) 0.0428(13) 0.0445(13) -0.0011(11) -0.0025(12) -0.0273(12)
C11 0.0408(14) 0.0566(16) 0.0485(15) -0.0030(13) 0.0055(12) -0.0257(13)
C12 0.0465(16) 0.0562(17) 0.0654(19) 0.0096(14) -0.0183(14) -0.0252(14)
C13 0.0473(15) 0.0291(13) 0.079(2) -0.0037(12) -0.0033(15) -0.0136(12)
C14 0.0441(15) 0.0455(16) 0.0674(19) -0.0014(13) 0.0141(14) -0.0092(13)
#==================================================================
# 10. MOLECULAR GEOMETRY
#===================================================================
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si N1 1.6554(19) . . yes
Si C12 1.871(4) . . yes
Si C13 1.877(3) . . yes
Si C14 1.880(4) . . yes
N1 C1 1.275(3) . . yes
N2 C1 1.394(2) . . yes
N2 C2 1.387(3) . . yes
N2 C4 1.491(3) . . yes
N3 C1 1.393(3) . . yes
N3 C3 1.387(3) . . yes
N3 C8 1.492(3) . . yes
C2 C3 1.326(4) . . no
C4 C5 1.527(4) . . no
C4 C6 1.527(4) . . no
C4 C7 1.532(3) . . no
C8 C9 1.527(4) . . no
C8 C10 1.528(3) . . no
C8 C11 1.528(4) . . no
C2 H21 0.96(3) . . no
C3 H31 0.94(4) . . no
C5 H51 0.98(3) . . no
C5 H52 0.98(3) . . no
C5 H53 1.00(4) . . no
C6 H61 0.95(3) . . no
C6 H62 0.98(3) . . no
C6 H63 0.99(3) . . no
C7 H71 0.98(3) . . no
C7 H72 0.95(4) . . no
C7 H73 0.99(3) . . no
C9 H91 0.96(3) . . no
C9 H92 1.05(3) . . no
C9 H93 0.97(3) . . no
C10 H101 0.98(4) . . no
C10 H102 1.02(4) . . no
C10 H103 0.96(3) . . no
C11 H111 0.97(4) . . no
C11 H112 0.98(4) . . no
C11 H113 1.04(3) . . no
C12 H121 0.95(4) . . no
C12 H122 0.97(4) . . no
C12 H123 0.97(5) . . no
C13 H131 1.05(5) . . no
C13 H132 1.03(4) . . no
C13 H133 0.96(4) . . no
C14 H141 1.08(3) . . no
C14 H142 1.02(4) . . no
C14 H143 1.03(4) . . no
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Si C12 110.96(13) . . . yes
N1 Si C13 112.26(13) . . . yes
N1 Si C14 112.85(13) . . . yes
C12 Si C13 107.84(15) . . . yes
C12 Si C14 106.34(17) . . . yes
C13 Si C14 106.24(15) . . . yes
Si N1 C1 169.33(18) . . . yes
C1 N2 C2 109.2(2) . . . yes
C1 N2 C4 125.05(19) . . . yes
C2 N2 C4 125.74(19) . . . yes
C1 N3 C3 109.39(18) . . . yes
C1 N3 C8 125.12(18) . . . yes
C3 N3 C8 125.4(2) . . . yes
N1 C1 N2 127.8(2) . . . yes
N1 C1 N3 127.65(19) . . . yes
N2 C1 N3 104.52(17) . . . yes
N2 C2 C3 108.6(2) . . . yes
N3 C3 C2 108.3(2) . . . yes
N2 C4 C5 109.4(2) . . . yes
N2 C4 C6 109.26(18) . . . yes
N2 C4 C7 109.0(2) . . . yes
C5 C4 C6 108.9(2) . . . no
C5 C4 C7 108.5(2) . . . no
C6 C4 C7 111.8(2) . . . no
N3 C8 C9 109.5(2) . . . yes
N3 C8 C10 108.91(17) . . . yes
N3 C8 C11 109.0(2) . . . yes
C9 C8 C10 112.1(2) . . . no
C9 C8 C11 108.3(2) . . . no
C10 C8 C11 109.1(2) . . . no
N2 C2 H21 123.1(18) . . . no
C3 C2 H21 128.2(18) . . . no
N3 C3 H31 122.5(17) . . . no
C2 C3 H31 129.2(17) . . . no
C4 C5 H51 110(2) . . . no
C4 C5 H52 109.3(15) . . . no
C4 C5 H53 109(2) . . . no
H51 C5 H52 108(3) . . . no
H51 C5 H53 112(3) . . . no
H52 C5 H53 108(2) . . . no
C4 C6 H61 111(2) . . . no
C4 C6 H62 111.9(17) . . . no
C4 C6 H63 109.5(15) . . . no
H61 C6 H62 106(2) . . . no
H61 C6 H63 108(2) . . . no
H62 C6 H63 110(2) . . . no
C4 C7 H71 111.2(14) . . . no
C4 C7 H72 111.1(18) . . . no
C4 C7 H73 108.5(14) . . . no
H71 C7 H72 108(2) . . . no
H71 C7 H73 109(2) . . . no
H72 C7 H73 108(3) . . . no
C8 C9 H91 114.6(15) . . . no
C8 C9 H92 112(2) . . . no
C8 C9 H93 110.8(18) . . . no
H91 C9 H92 104(3) . . . no
H91 C9 H93 108(2) . . . no
H92 C9 H93 108(3) . . . no
C8 C10 H101 110.3(16) . . . no
C8 C10 H102 111.5(19) . . . no
C8 C10 H103 108(2) . . . no
H101 C10 H102 111(3) . . . no
H101 C10 H103 107(3) . . . no
H102 C10 H103 109(2) . . . no
C8 C11 H111 110(2) . . . no
C8 C11 H112 109(2) . . . no
C8 C11 H113 108.7(18) . . . no
H111 C11 H112 112(3) . . . no
H111 C11 H113 111(2) . . . no
H112 C11 H113 106(3) . . . no
Si C12 H121 110(2) . . . no
Si C12 H122 115(2) . . . no
Si C12 H123 111(2) . . . no
H121 C12 H122 113(3) . . . no
H121 C12 H123 104(4) . . . no
H122 C12 H123 103(3) . . . no
Si C13 H131 100(2) . . . no
Si C13 H132 108.7(19) . . . no
Si C13 H133 112(2) . . . no
H131 C13 H132 110(3) . . . no
H131 C13 H133 116(3) . . . no
H132 C13 H133 110(3) . . . no
Si C14 H141 106.8(14) . . . no
Si C14 H142 112(2) . . . no
Si C14 H143 110(2) . . . no
H141 C14 H142 117(3) . . . no
H141 C14 H143 110(2) . . . no
H142 C14 H143 101(3) . . . no
# CIF-file generated for RANF 4332-173
# Compound 5
#===================================================================
data_RANF-4332-173
_database_code_depnum_ccdc_archive 'CCDC 229689'
#===================================================================
_audit_creation_date 13-Jan-04
_audit_creation_method 'PLATON option'
_audit_update_record
;
13-Jan-04 Updated by the Author E.H.
Textwriting by E.H.
Checkcif OK
14-Jan-04 Updated by the Author E.H.
20-Jan-04 Updated by the Author E.H.
;
#===================================================================
# 5. CHEMICAL DATA
#===================================================================
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_formula_moiety 'C16 H25 Cl2 N3 Ti'
_chemical_formula_structural ?
_chemical_formula_analytical ?
_chemical_formula_sum 'C16 H25 Cl2 N3 Ti'
_chemical_formula_weight 378.16
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#===================================================================
# 6. CRYSTAL DATA
#===================================================================
_symmetry_cell_setting Orthorhombic
_symmetry_space_group_name_Hall '-P 2ac 2n'
_symmetry_space_group_name_H-M 'P n m a'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,-y,1/2+z
1/2+x,1/2-y,1/2-z
-x,1/2+y,-z
-x,-y,-z
1/2+x,y,1/2-z
1/2-x,1/2+y,1/2+z
x,1/2-y,z
_cell_length_a 12.8780(2)
_cell_length_b 17.5935(2)
_cell_length_c 8.5676(1)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 1941.15(4)
_cell_formula_units_Z 4
_cell_measurement_temperature 173(1)
_cell_measurement_reflns_used 2077
_cell_measurement_theta_min 2.64
_cell_measurement_theta_max 25.36
_exptl_crystal_description fragment
_exptl_crystal_colour red
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.08
_exptl_crystal_density_meas none
_exptl_crystal_density_diffrn 1.294
_exptl_crystal_density_method none
_exptl_crystal_F_000 792
_exptl_absorpt_coefficient_mu 0.716
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.870
_exptl_absorpt_correction_T_max 0.945
_exptl_absorpt_process_details
'(applied during the scaling procedure; Nonius, 2001b)'
_exptl_special_details
;
Diffractometer operator E. Herdtweck
scanspeed 2 x 120 s per film
repetition 1
dx 40
467 films measured in 8 data sets
set 1: phi-scan with delta_phi = 2.0
set 2 to 8 omega-scans with delta_omega = 2.0
;
_publ_section_exptl_prep
;
The crystal was fixed in a capillary with perfluorinated ether and
transferred to the diffractometer.
;
_publ_section_exptl_refinement
;
Straight forward after integration with the program NPROCESS,
source: Nonius (2001b).
Hydrogen atoms could be located in the difference Fourier maps
and refined freely.
;
#===================================================================
# 7. EXPERIMENTAL DATA
#===================================================================
_diffrn_ambient_temperature 173(1)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_source 'NONIUS FR 591 rotating anode'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device ' \k-geometry diffractometer '
_diffrn_measurement_device_type ' Nonius \k-CCD diffractometer'
_diffrn_measurement_method ' phi- and omega-rotation '
_diffrn_detector ' CCD plate '
_diffrn_detector_area_resol_mean 18 # 9 for binned mode
_diffrn_standards_decay_% 0
# number of measured reflections (redundant set)
_diffrn_reflns_number 40109
_diffrn_reflns_av_R_equivalents 0.050
_diffrn_reflns_av_sigmaI/netI 0.0190
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_l_min -10
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_theta_min 2.64
_diffrn_reflns_theta_max 25.36
_reflns_number_total 1848
_reflns_number_gt 1665
# number of observed reflections (> n sig(I))
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'Kappa-CCD Control Software (Nonius, 2001a)'
_computing_cell_refinement 'DENZO (Nonius, 2001b)'
_computing_data_reduction 'DENZO (Nonius, 2001b)'
_computing_structure_solution 'SIR92 (Altomare, 1994)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)'
_computing_molecular_graphics 'PLATON (Spek, 2001)'
_computing_publication_material 'PLATON (Spek, 2001)'
#===================================================================
# 8. REFINEMENT DATA
#===================================================================
_refine_special_details
;
Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^
or flagged by the user for potential systematic errors. Weighted R-factors
wR and all goodnesses of fit S are based on F^2^, conventional R-factors R
are based on F, with F set to zero for negative F^2^. The observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme sigma
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(Fo^2^)+(0.0303P)^2^+1.9495P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_ls_hydrogen_treatment refall
_refine_ls_number_reflns 1848
_refine_ls_number_parameters 157
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0403
_refine_ls_R_factor_gt 0.0347
_refine_ls_wR_factor_ref 0.0901
_refine_ls_wR_factor_gt 0.0877
_refine_ls_goodness_of_fit_ref 1.212
_refine_ls_restrained_S_all 1.212
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 25.36
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 0.450
_refine_diff_density_min -0.278
_refine_diff_density_rms 0.053
#===================================================================
# 9. ATOMIC COORDINATES AND THERMAL PARAMETERS
#===================================================================
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
Ti Ti Uani 0.53120(4) 0.25000 -0.17713(6) 1.000 0.0225(2) . .
Cl Cl Uani 0.64044(4) 0.14721(3) -0.13078(7) 1.000 0.0328(2) . .
N1 N Uani 0.44773(19) 0.25000 -0.0137(3) 1.000 0.0220(8) . .
N2 N Uani 0.32700(14) 0.18761(10) 0.1607(2) 1.000 0.0240(6) . .
C1 C Uani 0.3723(2) 0.25000 0.0927(3) 1.000 0.0209(9) . .
C2 C Uani 0.25495(18) 0.21216(14) 0.2691(3) 1.000 0.0293(7) . .
C3 C Uani 0.35598(18) 0.10603(13) 0.1363(3) 1.000 0.0285(7) . .
C4 C Uani 0.2832(3) 0.05691(17) 0.2335(5) 1.000 0.0539(13) . .
C5 C Uani 0.4669(2) 0.09464(16) 0.1924(3) 1.000 0.0375(9) . .
C6 C Uani 0.3449(2) 0.08519(16) -0.0351(3) 1.000 0.0386(9) . .
C7 C Uani 0.3905(4) 0.25000 -0.3495(5) 1.000 0.0633(19) . .
C8 C Uani 0.4470(3) 0.1871(2) -0.3831(4) 1.000 0.0625(15) . .
C9 C Uani 0.5414(3) 0.2110(2) -0.4468(3) 1.000 0.0613(13) . .
H21 H Uiso 0.216(2) 0.1799(15) 0.327(3) 1.000 0.032(7) . .
H41 H Uiso 0.293(3) 0.0694(19) 0.348(4) 1.000 0.061(10) . .
H42 H Uiso 0.212(3) 0.0619(18) 0.200(4) 1.000 0.057(10) . .
H43 H Uiso 0.301(2) 0.009(2) 0.218(4) 1.000 0.053(9) . .
H51 H Uiso 0.471(2) 0.1063(18) 0.301(4) 1.000 0.054(9) . .
H52 H Uiso 0.488(2) 0.0438(19) 0.184(3) 1.000 0.053(9) . .
H53 H Uiso 0.515(2) 0.1280(18) 0.134(3) 1.000 0.045(8) . .
H61 H Uiso 0.393(2) 0.1105(17) -0.100(3) 1.000 0.043(8) . .
H62 H Uiso 0.355(2) 0.0309(18) -0.047(4) 1.000 0.050(8) . .
H63 H Uiso 0.276(3) 0.0975(19) -0.071(4) 1.000 0.067(10) . .
H71 H Uiso 0.309(5) 0.25000 -0.305(7) 1.000 0.10(2) . .
H81 H Uiso 0.431(3) 0.133(2) -0.367(4) 1.000 0.080(12) . .
H91 H Uiso 0.594(3) 0.181(2) -0.470(5) 1.000 0.088(13) . .
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
Ti 0.0175(3) 0.0325(3) 0.0175(3) 0.0000 0.0015(2) 0.0000
Cl 0.0284(3) 0.0336(3) 0.0365(3) -0.0056(3) 0.0023(2) 0.0073(2)
N1 0.0216(13) 0.0225(13) 0.0220(13) 0.0000 0.0035(11) 0.0000
N2 0.0261(10) 0.0204(9) 0.0256(10) -0.0010(8) 0.0073(8) -0.0013(8)
C1 0.0220(15) 0.0222(15) 0.0186(15) 0.0000 0.0011(12) 0.0000
C2 0.0296(12) 0.0292(12) 0.0292(12) 0.0021(10) 0.0109(10) -0.0024(10)
C3 0.0323(13) 0.0176(11) 0.0355(13) -0.0016(10) 0.0077(10) -0.0004(10)
C4 0.062(2) 0.0218(15) 0.078(3) 0.0008(15) 0.034(2) -0.0046(14)
C5 0.0462(16) 0.0301(15) 0.0362(15) 0.0006(12) -0.0028(13) 0.0082(13)
C6 0.0422(16) 0.0302(15) 0.0435(16) -0.0125(12) -0.0030(13) -0.0041(12)
C7 0.033(2) 0.126(5) 0.031(2) 0.0000 -0.0088(18) 0.0000
C8 0.082(3) 0.077(3) 0.0285(15) -0.0069(16) -0.0198(17) -0.026(2)
C9 0.0557(19) 0.107(3) 0.0212(13) -0.0197(15) -0.0048(13) 0.0243(18)
#==================================================================
# 10. MOLECULAR GEOMETRY
#===================================================================
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti Cl 2.3253(6) . . yes
Ti N1 1.765(3) . . yes
Ti C7 2.338(5) . . yes
Ti C8 2.348(4) . . yes
Ti C9 2.414(3) . . yes
N1 C1 1.332(4) . . yes
N2 C1 1.373(2) . . yes
N2 C2 1.382(3) . . yes
N2 C3 1.498(3) . . yes
C2 C2 1.331(3) . 8_555 no
C3 C4 1.523(4) . . no
C3 C5 1.520(3) . . no
C3 C6 1.520(4) . . no
C7 C8 1.355(5) . . no
C8 C9 1.397(5) . . no
C9 C9 1.372(5) . 8_555 no
C2 H21 0.91(3) . . no
C4 H41 1.01(3) . . no
C4 H42 0.96(4) . . no
C4 H43 0.88(3) . . no
C5 H51 0.95(3) . . no
C5 H52 0.94(3) . . no
C5 H53 0.99(3) . . no
C6 H61 0.94(3) . . no
C6 H62 0.97(3) . . no
C6 H63 0.96(4) . . no
C7 H71 1.12(6) . . no
C8 H81 0.98(4) . . no
C9 H91 0.88(4) . . no
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl Ti N1 103.47(5) . . . yes
Cl Ti C7 125.23(4) . . . yes
Cl Ti C8 92.36(9) . . . yes
Cl Ti C9 84.81(9) . . . yes
Cl Ti Cl 102.10(3) . . 8_555 yes
Cl Ti C8 140.73(9) . . 8_555 yes
Cl Ti C9 110.59(9) . . 8_555 yes
N1 Ti C7 91.67(14) . . . yes
N1 Ti C8 108.35(12) . . . yes
N1 Ti C9 142.41(12) . . . yes
Cl Ti N1 103.47(5) 8_555 . . yes
N1 Ti C8 108.35(12) . . 8_555 yes
N1 Ti C9 142.41(12) . . 8_555 yes
C7 Ti C8 33.62(11) . . . yes
C7 Ti C9 55.77(14) . . . yes
Cl Ti C7 125.23(4) 8_555 . . yes
C7 Ti C8 33.62(11) . . 8_555 yes
C7 Ti C9 55.77(14) . . 8_555 yes
C8 Ti C9 34.09(13) . . . yes
Cl Ti C8 140.73(9) 8_555 . . yes
C8 Ti C8 56.23(12) . . 8_555 yes
C8 Ti C9 55.93(12) . . 8_555 yes
Cl Ti C9 110.59(9) 8_555 . . yes
C8 Ti C9 55.93(12) 8_555 . . yes
C9 Ti C9 33.03(12) . . 8_555 yes
Cl Ti C8 92.36(9) 8_555 . 8_555 yes
Cl Ti C9 84.81(9) 8_555 . 8_555 yes
C8 Ti C9 34.09(13) 8_555 . 8_555 yes
Ti N1 C1 170.7(2) . . . yes
C1 N2 C2 108.70(18) . . . yes
C1 N2 C3 126.95(18) . . . yes
C2 N2 C3 124.10(19) . . . yes
N1 C1 N2 126.89(11) . . . yes
N1 C1 N2 126.89(11) . . 8_555 yes
N2 C1 N2 106.2(2) . . 8_555 yes
N2 C2 C2 108.2(2) . . 8_555 yes
N2 C3 C4 108.3(2) . . . yes
N2 C3 C5 108.44(19) . . . yes
N2 C3 C6 110.0(2) . . . yes
C4 C3 C5 109.3(2) . . . no
C4 C3 C6 109.5(2) . . . no
C5 C3 C6 111.2(2) . . . no
Ti C7 C8 73.6(3) . . . yes
Ti C7 C8 73.6(3) . . 8_555 yes
C8 C7 C8 109.5(4) . . 8_555 no
Ti C8 C7 72.8(2) . . . yes
Ti C8 C9 75.52(19) . . . yes
C7 C8 C9 107.7(3) . . . no
Ti C9 C8 70.39(18) . . . yes
Ti C9 C9 73.48(16) . . 8_555 yes
C8 C9 C9 107.5(3) . . 8_555 no
N2 C2 H21 123.0(17) . . . no
C2 C2 H21 128.8(17) 8_555 . . no
C3 C4 H41 109(2) . . . no
C3 C4 H42 112(2) . . . no
C3 C4 H43 107(2) . . . no
H41 C4 H42 113(3) . . . no
H41 C4 H43 109(3) . . . no
H42 C4 H43 107(3) . . . no
C3 C5 H51 109.4(16) . . . no
C3 C5 H52 111.9(16) . . . no
C3 C5 H53 110.5(15) . . . no
H51 C5 H52 105(2) . . . no
H51 C5 H53 109(2) . . . no
H52 C5 H53 110(2) . . . no
C3 C6 H61 113.2(16) . . . no
C3 C6 H62 109(2) . . . no
C3 C6 H63 110(2) . . . no
H61 C6 H62 108(2) . . . no
H61 C6 H63 108(3) . . . no
H62 C6 H63 108(3) . . . no
Ti C7 H71 121(3) . . . no
C8 C7 H71 125.2(2) . . . no
C8 C7 H71 125.2(2) 8_555 . . no
Ti C8 H81 117(2) . . . no
C7 C8 H81 130(2) . . . no
C9 C8 H81 122(2) . . . no
Ti C9 H91 115(3) . . . no
C8 C9 H91 125(2) . . . no
C9 C9 H91 127(2) 8_555 . . no
# End of Crystallographic Information File