data_global
_journal_name_full               'Green Chemistry'

_journal_coden_Cambridge         1048

_publ_contact_author_name        "Dermot O'Hare"
_publ_contact_author_email       DERMOT.OHARE@CHEM.OX.AC.UK

_publ_section_title              
;
Catalytic dechlorination of polychlorinated
biphenyls (PCBs) using amine functionalised titanocenes
;
loop_
_publ_author_name
"Dermot O'Hare"
'Andrew E.D. Fletcher'
'Jonathan D. Hyatt'
'Kang Min Ok.'

# Attachment 'Structure__4_-new.cif'

#\#CIF_1.1

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2007-03-30 at 09:57:22
# Using CIFtbx version 2.6.2 16 Jun 1998

# Dictionary name : cif_core.dic
# Dictionary vers : 2.3
# Request file : c:\wingx\files\archive.dat
# CIF files read : jh2

data_jh2
_database_code_depnum_ccdc_archive 'CCDC 725827'

_audit_creation_date             2007-03-30T09:57:22-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        ?
_chemical_name_common            N/A
_chemical_formula_sum            'C11 H17 Cl2 N Ti'
_chemical_formula_weight         282.06

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   7.3084(15)
_cell_length_b                   10.576(2)
_cell_length_c                   8.5363(17)
_cell_angle_alpha                90
_cell_angle_beta                 102.70(3)
_cell_angle_gamma                90
_cell_volume                     643.7(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.0(2)

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             292
_exptl_special_details           
;
?
;

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.048
_exptl_absorpt_correction_type   none
_exptl_crystal_recrystallization_method toluene
_exptl_crystal_description       Prism
_exptl_crystal_colour            Red
_exptl_crystal_size_min          0.06
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_max          0.26

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      150.0(2)
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_reflns_av_R_equivalents  0.018
_diffrn_reflns_av_unetI/netI     0.026
_diffrn_reflns_number            2695
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         6.02
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_full        27.5
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_reflns_number_total             1534
_reflns_number_gt                1307
_reflns_threshold_expression     >3\(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness 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 threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+0.5743P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_coef       0.010(7)
_refine_ls_number_reflns         1534
_refine_ls_number_parameters     89
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0393
_refine_ls_wR_factor_ref         0.1042
_refine_ls_wR_factor_gt          0.0975
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.062

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 '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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.34095(7) 0.25 0.09680(6) 0.0287(2) Uani 1 2 d S . .
Cl1 Cl 0.20053(9) 0.07815(6) 0.18305(9) 0.0502(2) Uani 1 1 d . . .
N1 N 0.5983(4) 0.25 0.2025(3) 0.0428(7) Uani 1 2 d S . .
C1 C 0.1970(3) 0.1837(2) -0.1654(3) 0.0414(6) Uani 1 1 d . . .
H1 H 0.089 0.1307 -0.1845 0.05 Uiso 1 1 calc R . .
C2 C 0.3851(3) 0.1430(2) -0.1320(3) 0.0365(5) Uani 1 1 d . . .
H2 H 0.4246 0.061 -0.1252 0.044 Uiso 1 1 calc R . .
C3 C 0.5018(4) 0.25 -0.1110(4) 0.0331(7) Uani 1 2 d S . .
C4 C 0.7089(4) 0.25 -0.0451(4) 0.0506(10) Uani 1 2 d S . .
H4A H 0.7686 0.1936 -0.1084 0.061 Uiso 0.5 1 calc PR . .
H4B H 0.7579 0.3344 -0.053 0.061 Uiso 0.5 1 calc PR . .
C5 C 0.7529(5) 0.2103(4) 0.1186(5) 0.0303(9) Uani 0.5 1 d P . -1
H5A H 0.8709 0.2477 0.1731 0.036 Uiso 1 2 calc SR . -1
H5B H 0.7668 0.1191 0.1236 0.036 Uiso 0.5 1 calc PR . -1
C6 C 0.6678(5) 0.25 0.3830(4) 0.0479(9) Uani 1 2 d S . .
C7 C 0.7857(5) 0.1323(3) 0.4331(4) 0.0653(9) Uani 1 1 d . . .
H7A H 0.893 0.1339 0.386 0.098 Uiso 1 1 calc R . .
H7B H 0.712 0.0584 0.397 0.098 Uiso 1 1 calc R . .
H7C H 0.826 0.1304 0.548 0.098 Uiso 1 1 calc R . .
C8 C 0.5056(7) 0.25 0.4672(5) 0.113(3) Uani 1 2 d S . .
H8A H 0.446 0.323 0.450 0.169 Uiso 0.5 1 calc PR . .
H8B H 0.549 0.239 0.571 0.169 Uiso 0.5 1 calc PR . .
H8C H 0.428 0.188 0.429 0.169 Uiso 0.5 1 calc PR . .

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 0.0212(3) 0.0329(3) 0.0330(3) 0 0.0079(2) 0
Cl1 0.0510(4) 0.0404(4) 0.0658(5) 0.0131(3) 0.0274(3) 0.0002(3)
N1 0.0236(12) 0.080(2) 0.0262(13) 0 0.0080(10) 0
C1 0.0370(11) 0.0456(13) 0.0369(12) -0.0042(10) -0.0021(9) -0.0109(10)
C2 0.0458(12) 0.0306(11) 0.0323(11) -0.0037(9) 0.0068(9) 0.0029(10)
C3 0.0305(14) 0.0444(17) 0.0261(14) 0 0.0098(11) 0
C4 0.0241(15) 0.092(3) 0.0388(18) 0 0.0132(13) 0
C5 0.0209(16) 0.035(2) 0.035(2) 0.0000(15) 0.0067(15) 0.0000(13)
C6 0.0360(17) 0.080(3) 0.0253(15) 0 0.0023(13) 0
C7 0.089(2) 0.0598(18) 0.0404(14) 0.0057(14) -0.0001(15) -0.0041(17)
C8 0.056(3) 0.258(11) 0.029(2) 0 0.018(2) 0

#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 N1 1.899(3) . ?
Ti1 Cl1 2.2871(8) 4_565 ?
Ti1 Cl1 2.2871(8) . ?
Ti1 C3 2.334(3) . ?
Ti1 C2 2.340(2) . ?
Ti1 C2 2.340(2) 4_565 ?
Ti1 C1 2.360(2) . ?
Ti1 C1 2.360(2) 4_565 ?
N1 C6 1.513(4) . ?
N1 C5 1.524(5) . ?
N1 C5 1.524(5) 4_565 ?
C1 C1 1.402(5) 4_565 ?
C1 C2 1.409(3) . ?
C2 C3 1.405(3) . ?
C3 C2 1.405(3) 4_565 ?
C3 C4 1.494(4) . ?
C4 C5 1.426(5) 4_565 ?
C4 C5 1.426(5) . ?
C6 C8 1.516(6) . ?
C6 C7 1.520(4) 4_565 ?
C6 C7 1.520(4) . ?

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_3
_geom_angle_publ_flag
N1 Ti1 Cl1 108.35(5) . 4_565 ?
N1 Ti1 Cl1 108.35(5) . . ?
Cl1 Ti1 Cl1 105.25(4) 4_565 . ?
N1 Ti1 C3 75.47(11) . . ?
Cl1 Ti1 C3 125.55(3) 4_565 . ?
Cl1 Ti1 C3 125.55(3) . . ?
N1 Ti1 C2 95.31(9) . . ?
Cl1 Ti1 C2 143.80(7) 4_565 . ?
Cl1 Ti1 C2 92.19(7) . . ?
C3 Ti1 C2 34.99(7) . . ?
N1 Ti1 C2 95.31(9) . 4_565 ?
Cl1 Ti1 C2 92.19(7) 4_565 4_565 ?
Cl1 Ti1 C2 143.80(7) . 4_565 ?
C3 Ti1 C2 34.99(7) . 4_565 ?
C2 Ti1 C2 57.85(12) . 4_565 ?
N1 Ti1 C1 129.70(10) . . ?
Cl1 Ti1 C1 113.78(7) 4_565 . ?
Cl1 Ti1 C1 86.06(7) . . ?
C3 Ti1 C1 58.21(9) . . ?
C2 Ti1 C1 34.87(8) . . ?
C2 Ti1 C1 57.78(9) 4_565 . ?
N1 Ti1 C1 129.70(10) . 4_565 ?
Cl1 Ti1 C1 86.06(7) 4_565 4_565 ?
Cl1 Ti1 C1 113.78(7) . 4_565 ?
C3 Ti1 C1 58.21(9) . 4_565 ?
C2 Ti1 C1 57.78(9) . 4_565 ?
C2 Ti1 C1 34.87(8) 4_565 4_565 ?
C1 Ti1 C1 34.55(13) . 4_565 ?
C6 N1 C5 111.2(3) . . ?
C6 N1 C5 111.2(3) . 4_565 ?
C5 N1 C5 32.0(3) . 4_565 ?
C6 N1 Ti1 124.0(2) . . ?
C5 N1 Ti1 122.4(2) . . ?
C5 N1 Ti1 122.4(2) 4_565 . ?
C1 C1 C2 107.82(14) 4_565 . ?
C1 C1 Ti1 72.73(6) 4_565 . ?
C2 C1 Ti1 71.79(13) . . ?
C3 C2 C1 108.5(2) . . ?
C3 C2 Ti1 72.24(15) . . ?
C1 C2 Ti1 73.35(14) . . ?
C2 C3 C2 107.3(3) 4_565 . ?
C2 C3 C4 125.76(14) 4_565 . ?
C2 C3 C4 125.76(14) . . ?
C2 C3 Ti1 72.77(15) 4_565 . ?
C2 C3 Ti1 72.77(15) . . ?
C4 C3 Ti1 110.6(2) . . ?
C5 C4 C5 34.3(3) 4_565 . ?
C5 C4 C3 111.1(3) 4_565 . ?
C5 C4 C3 111.1(3) . . ?
C4 C5 N1 110.4(3) . . ?
N1 C6 C8 111.1(3) . . ?
N1 C6 C7 109.2(2) . 4_565 ?
C8 C6 C7 108.7(2) . 4_565 ?
N1 C6 C7 109.2(2) . . ?
C8 C6 C7 108.7(2) . . ?
C7 C6 C7 109.9(3) 4_565 . ?
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'P 21/m'
_symmetry_int_tables_number      11
_chemical_absolute_configuration ?