#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/25/4072590.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4072590
loop_
_publ_author_name
'Owen, Christopher T.'
'Bolton, Paul D.'
'Cowley, Andrew R.'
'Mountford, Philip'
_publ_section_title
;
 Cyclopentadienyl Titanium Imido Compounds and Their Ethylene
 Polymerization Capability:  Control of Molecular Weight
 Distributions by Imido N-Substituents
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              83
_journal_paper_doi               10.1021/om0608556
_journal_volume                  26
_journal_year                    2007
_chemical_compound_source
;
synthesis as described
;
_chemical_formula_moiety         ' C22 H19 Cl2 F3 N4 Ti1 '
_chemical_formula_sum            'C22 H19 Cl2 F3 N4 Ti'
_chemical_formula_weight         515.22
_chemical_name_systematic
;                                      
Ti(N-2-C6H4CF3)Cl2(py)3
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 93.795(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4719(4)
_cell_length_b                   19.5247(8)
_cell_length_c                   9.6046(3)
_cell_measurement_reflns_used    9008
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     2333.69(14)
_computing_cell_refinement
; 
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) 
;
_computing_data_collection
; 
KappaCCD software 'Collect' (Nonius, 2000) 
;
_computing_data_reduction
; 
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) 
;
_computing_publication_material
; 
CRYSTALS (Watkin et al, 2001) 
;
_computing_structure_refinement
; 
CRYSTALS (Watkin et al, 2001) 
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
; 
Nonius KappaCCD 
;
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9008
_diffrn_reflns_theta_full        27.491
_diffrn_reflns_theta_max         27.491
_diffrn_reflns_theta_min         5.309
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.637
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_exptl_crystal_colour            ' yellow-brown '
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       ' fragment '
_exptl_crystal_F_000             1048.000
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.20
_refine_diff_density_min         -0.29
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1341
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         1807
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          0.006384
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.259 0.773E-01 0.392E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0592
_refine_ls_wR_factor_gt          0.0324
_refine_ls_wR_factor_ref         0.0324
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                1807
_reflns_number_total             2650
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            om0608556si20060918_031255.cif
_cod_data_source_block           COMPOUND_6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        ' C22 H19 Cl2 F3 N4 Ti1 '
_cod_database_code               4072590
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y,-z+1/2
x,-y,z+1/2
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2
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
_atom_site_disorder_group
Ti1 Ti 0.5000 0.20727(3) 0.2500 0.0249 1.0000 Uani ST .
Cl1 Cl 0.42738(4) 0.19090(3) 0.01571(5) 0.0362 1.0000 Uani . .
N1 N 0.5000 0.29586(12) 0.2500 0.0262 1.0000 Uani ST .
C1 C 0.5262(3) 0.3642(2) 0.2652(6) 0.0301 0.5000 Uani . -1
C2 C 0.6150(6) 0.3815(4) 0.3573(8) 0.0436 0.5000 Uani . -1
C3 C 0.6494(6) 0.4490(5) 0.3726(9) 0.0649 0.5000 Uani . -1
C4 C 0.5953(6) 0.5001(3) 0.3003(8) 0.0778 0.5000 Uani . -1
C5 C 0.5061(12) 0.4854(2) 0.2146(7) 0.0647 0.5000 Uani . -1
C6 C 0.4701(4) 0.4186(2) 0.1969(5) 0.0390 0.5000 Uani . -1
C7 C 0.3706(6) 0.4053(4) 0.1048(7) 0.0366 0.5000 Uani . -1
F1 F 0.3280(3) 0.46229(19) 0.0471(5) 0.0693 0.5000 Uani . -1
F2 F 0.2919(2) 0.37699(16) 0.1744(3) 0.0528 0.5000 Uani . -1
F3 F 0.3855(2) 0.36300(18) -0.0008(3) 0.0590 0.5000 Uani . -1
N2 N 0.5000 0.08538(12) 0.2500 0.0313 1.0000 Uani ST .
C8 C 0.41464(19) 0.04947(12) 0.1979(3) 0.0439 1.0000 Uani . .
C9 C 0.4110(3) -0.02121(14) 0.1983(3) 0.0641 1.0000 Uani . .
C10 C 0.5000 -0.0571(2) 0.2500 0.0711 1.0000 Uani ST .
N3 N 0.33499(12) 0.19247(8) 0.32077(16) 0.0265 1.0000 Uani . .
C11 C 0.31529(17) 0.15642(12) 0.4355(2) 0.0361 1.0000 Uani . .
C12 C 0.21377(18) 0.15042(13) 0.4838(2) 0.0406 1.0000 Uani . .
C13 C 0.12874(17) 0.18265(12) 0.4132(2) 0.0387 1.0000 Uani . .
C14 C 0.14781(16) 0.21877(12) 0.2939(2) 0.0380 1.0000 Uani . .
C15 C 0.25075(16) 0.22258(11) 0.2508(2) 0.0306 1.0000 Uani . .
H21 H 0.6539 0.3447 0.4125 0.0521 0.5000 Uiso . -1
H31 H 0.7137 0.4601 0.4364 0.0770 0.5000 Uiso . -1
H41 H 0.6210 0.5485 0.3101 0.0921 0.5000 Uiso . -1
H51 H 0.4664 0.5234 0.1641 0.0770 0.5000 Uiso . -1
H81 H 0.3507 0.0751 0.1568 0.0527 1.0000 Uiso . .
H91 H 0.3448 -0.0459 0.1617 0.0774 1.0000 Uiso . .
H101 H 0.5000 -0.1083 0.2500 0.0864 1.0000 Uiso . .
H111 H 0.3767 0.1330 0.4882 0.0436 1.0000 Uiso . .
H121 H 0.2023 0.1229 0.5693 0.0492 1.0000 Uiso . .
H131 H 0.0548 0.1800 0.4474 0.0471 1.0000 Uiso . .
H141 H 0.0873 0.2420 0.2391 0.0459 1.0000 Uiso . .
H151 H 0.2634 0.2488 0.1640 0.0368 1.0000 Uiso . .
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_IV_Table_2.2B
'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_IV_Table_2.2B
'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_IV_Table_2.2B
'F   ' 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 International_Tables_Vol_IV_Table_2.2B
'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_IV_Table_2.2B
'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_IV_Table_2.2B
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 . Ti1 Cl1 5_655 164.64(3) yes
Cl1 . Ti1 N1 . 97.681(17) yes
Cl1 5_655 Ti1 N1 . 97.681(17) yes
Cl1 . Ti1 N2 . 82.319(17) yes
Cl1 5_655 Ti1 N2 . 82.319(17) yes
N1 . Ti1 N2 . 179.995 yes
Cl1 . Ti1 N3 . 88.27(4) yes
Cl1 5_655 Ti1 N3 . 89.74(4) yes
N1 . Ti1 N3 . 97.45(4) yes
N2 . Ti1 N3 . 82.55(4) yes
Cl1 . Ti1 N3 5_655 89.74(4) yes
Cl1 5_655 Ti1 N3 5_655 88.27(4) yes
N1 . Ti1 N3 5_655 97.45(4) yes
N2 . Ti1 N3 5_655 82.55(4) yes
N3 . Ti1 N3 5_655 165.10(8) yes
Ti1 . N1 C1 . 165.34(15) yes
N1 . C1 C2 . 118.0(4) yes
N1 . C1 C6 . 125.0(3) yes
C2 . C1 C6 . 117.0(5) yes
C1 . C2 C3 . 121.2(7) yes
C1 . C2 H21 . 119.405 no
C3 . C2 H21 . 119.402 no
C2 . C3 C4 . 119.9(7) yes
C2 . C3 H31 . 120.040 no
C4 . C3 H31 . 120.036 no
C3 . C4 C5 . 120.4(6) yes
C3 . C4 H41 . 119.794 no
C5 . C4 H41 . 119.797 no
C4 . C5 C6 . 120.9(8) yes
C4 . C5 H51 . 119.528 no
C6 . C5 H51 . 119.524 no
C1 . C6 C5 . 120.4(6) yes
C1 . C6 C7 . 120.7(5) yes
C5 . C6 C7 . 119.0(7) yes
C6 . C7 F1 . 113.1(6) yes
C6 . C7 F2 . 112.5(5) yes
F1 . C7 F2 . 105.4(5) yes
C6 . C7 F3 . 113.9(5) yes
F1 . C7 F3 . 105.8(5) yes
F2 . C7 F3 . 105.5(5) yes
Ti1 . N2 C8 . 121.46(14) yes
Ti1 . N2 C8 5_655 121.46(14) yes
C8 . N2 C8 5_655 117.1(3) yes
N2 . C8 C9 . 123.1(3) yes
N2 . C8 H81 . 118.462 no
C9 . C8 H81 . 118.461 no
C8 . C9 C10 . 119.0(3) yes
C8 . C9 H91 . 120.525 no
C10 . C9 H91 . 120.524 no
C9 . C10 C9 5_655 118.8(4) yes
C9 . C10 H101 . 120.596 no
C9 5_655 C10 H101 . 120.596 no
Ti1 . N3 C11 . 122.73(13) yes
Ti1 . N3 C15 . 119.86(13) yes
C11 . N3 C15 . 117.35(17) yes
N3 . C11 C12 . 122.73(19) yes
N3 . C11 H111 . 118.636 no
C12 . C11 H111 . 118.636 no
C11 . C12 C13 . 119.4(2) yes
C11 . C12 H121 . 120.309 no
C13 . C12 H121 . 120.309 no
C12 . C13 C14 . 118.32(19) yes
C12 . C13 H131 . 120.839 no
C14 . C13 H131 . 120.839 no
C13 . C14 C15 . 119.52(19) yes
C13 . C14 H141 . 120.238 no
C15 . C14 H141 . 120.238 no
N3 . C15 C14 . 122.66(19) yes
N3 . C15 H151 . 118.667 no
C14 . C15 H151 . 118.668 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ti1 Cl1 . 2.3909(5) yes
Ti1 Cl1 5_655 2.3909(5) yes
Ti1 N1 . 1.730(2) yes
Ti1 N2 . 2.380(2) yes
Ti1 N3 . 2.2284(15) yes
Ti1 N3 5_655 2.2284(15) yes
N1 C1 . 1.378(4) yes
C1 C2 . 1.413(8) yes
C1 C6 . 1.410(6) yes
C2 C3 . 1.389(9) yes
C3 C4 . 1.369(11) yes
C4 C5 . 1.369(16) yes
C5 C6 . 1.387(7) yes
C6 C7 . 1.498(9) yes
C7 F1 . 1.337(8) yes
C7 F2 . 1.343(7) yes
C7 F3 . 1.330(8) yes
N2 C8 . 1.344(3) yes
N2 C8 5_655 1.344(3) yes
C8 C9 . 1.381(4) yes
C8 H81 . 1.000 no
C9 C10 . 1.377(4) yes
C9 H91 . 1.000 no
C10 H101 . 1.000 no
N3 C11 . 1.344(3) yes
N3 C15 . 1.344(3) yes
C11 C12 . 1.382(3) yes
C11 H111 . 1.000 no
C12 C13 . 1.373(3) yes
C12 H121 . 1.000 no
C13 C14 . 1.379(3) yes
C13 H131 . 1.000 no
C14 C15 . 1.377(3) yes
C14 H141 . 1.000 no
C15 H151 . 1.000 no
