#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:16:38 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179807 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/03/7010365.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_7010365
loop_
_publ_author_name
'Nielson, Alastair J.'
'Glenny, Mark W.'
'Rickard, Clifton E. F.'
_publ_section_title
;
 2-tert-Butyl and 2-phenylphenylimido complexes of titanium(IV) and
 their olefin polymerisation activity
;
_journal_issue                   3
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              232
_journal_paper_doi               10.1039/b008232p
_journal_year                    2001
_chemical_formula_moiety         'C40 H46 Cl4 N6 Ti2, 2(C H2 Cl2)'
_chemical_formula_sum            'C22 H27 Cl6 N3 Ti'
_chemical_formula_weight         594.07
_chemical_name_systematic
; 
 dichloro-di-μ-chloro(2-t-butylphenylimido)tetrakis-
pyridinedititanium(IV) bis(dichloromethane) solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.0130(10)
_cell_angle_beta                 77.1400(9)
_cell_angle_gamma                84.5900(10)
_cell_formula_units_Z            2
_cell_length_a                   8.042
_cell_length_b                   10.73410(10)
_cell_length_c                   16.4281(2)
_cell_measurement_reflns_used    5528
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     1345.73(2)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'Siemens SAINT  (Siemens, 1995)'
_computing_molecular_graphics    'Siemens SHELXTL (Siemens, 1994)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 Sheldrick, (1997)'
_computing_structure_solution    'SHELXS Sheldrick, (1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.887
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_device_type  'Siemens SMART'
_diffrn_measurement_method       'Area detector ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13769
_diffrn_reflns_theta_full        28.59
_diffrn_reflns_theta_max         28.59
_diffrn_reflns_theta_min         1.30
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.930
_exptl_absorpt_correction_T_max  0.8008
_exptl_absorpt_correction_T_min  0.7189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.992
_refine_diff_density_min         -1.210
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         6103
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0983P)²+1.0795P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1548
_refine_ls_wR_factor_ref         0.1615
_reflns_number_gt                5181
_reflns_number_total             6103
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b008232p.txt
_cod_data_source_block           '[4]'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' 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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0983P)^2^+1.0795P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0983P)^2^+1.0795P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1345.67(2)
_cod_database_code               7010365
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti Ti -0.01183(5) 0.64514(4) 0.40019(3) 0.02184(14) Uani 1 d . . .
Cl1 Cl -0.26178(8) 0.77633(6) 0.39435(4) 0.03260(17) Uani 1 d . . .
Cl2 Cl 0.18876(7) 0.47462(6) 0.44840(4) 0.02547(15) Uani 1 d . . .
N1 N 0.1234(3) 0.7087(2) 0.30768(13) 0.0253(4) Uani 1 d . . .
C1 C 0.2609(3) 0.7377(3) 0.24061(16) 0.0267(5) Uani 1 d . . .
C2 C 0.2574(3) 0.8353(3) 0.16745(16) 0.0282(5) Uani 1 d . . .
C3 C 0.4058(4) 0.8487(3) 0.10479(18) 0.0365(6) Uani 1 d . . .
H3 H 0.4061 0.9117 0.0547 0.044 Uiso 1 calc R . .
C4 C 0.5513(4) 0.7746(4) 0.1124(2) 0.0452(8) Uani 1 d . . .
H4 H 0.6485 0.7867 0.0679 0.054 Uiso 1 calc R . .
C5 C 0.5557(4) 0.6833(4) 0.1844(2) 0.0489(8) Uani 1 d . . .
H5 H 0.6566 0.6337 0.1909 0.059 Uiso 1 calc R . .
C6 C 0.4099(4) 0.6644(3) 0.2479(2) 0.0395(7) Uani 1 d . . .
H6 H 0.4120 0.6003 0.2972 0.047 Uiso 1 calc R . .
C7 C 0.0997(3) 0.9217(3) 0.15669(17) 0.0311(6) Uani 1 d . . .
C8 C 0.1314(5) 1.0246(4) 0.0747(2) 0.0486(8) Uani 1 d . . .
H8A H 0.0297 1.0802 0.0719 0.073 Uiso 1 calc R . .
H8B H 0.1587 0.9843 0.0258 0.073 Uiso 1 calc R . .
H8C H 0.2261 1.0745 0.0744 0.073 Uiso 1 calc R . .
C9 C -0.0452(4) 0.8420(3) 0.1543(2) 0.0394(7) Uani 1 d . . .
H9A H -0.1440 0.8978 0.1444 0.059 Uiso 1 calc R . .
H9B H -0.0748 0.7817 0.2084 0.059 Uiso 1 calc R . .
H9C H -0.0092 0.7955 0.1086 0.059 Uiso 1 calc R . .
C10 C 0.0465(4) 0.9915(3) 0.23019(19) 0.0369(6) Uani 1 d . . .
H10A H -0.0537 1.0470 0.2225 0.055 Uiso 1 calc R . .
H10B H 0.1391 1.0424 0.2313 0.055 Uiso 1 calc R . .
H10C H 0.0201 0.9295 0.2837 0.055 Uiso 1 calc R . .
N2 N -0.1165(3) 0.5087(2) 0.34515(14) 0.0280(4) Uani 1 d . . .
C21 C -0.2783(4) 0.4741(3) 0.36976(19) 0.0336(6) Uani 1 d . . .
H21 H -0.3489 0.5047 0.4156 0.040 Uiso 1 calc R . .
C22 C -0.3459(4) 0.3964(3) 0.3313(2) 0.0410(7) Uani 1 d . . .
H22 H -0.4601 0.3734 0.3508 0.049 Uiso 1 calc R . .
C23 C -0.2447(5) 0.3530(3) 0.2643(2) 0.0505(8) Uani 1 d . . .
H23 H -0.2888 0.3010 0.2358 0.061 Uiso 1 calc R . .
C24 C -0.0783(5) 0.3859(4) 0.2390(2) 0.0527(9) Uani 1 d . . .
H24 H -0.0055 0.3558 0.1935 0.063 Uiso 1 calc R . .
C25 C -0.0196(4) 0.4632(3) 0.2809(2) 0.0401(7) Uani 1 d . . .
H25 H 0.0952 0.4852 0.2633 0.048 Uiso 1 calc R . .
N3 N 0.0773(3) 0.7601(2) 0.47505(14) 0.0266(4) Uani 1 d . . .
C31 C 0.2418(3) 0.7873(3) 0.45807(18) 0.0328(6) Uani 1 d . . .
H31 H 0.3172 0.7555 0.4140 0.039 Uiso 1 calc R . .
C32 C 0.3048(4) 0.8591(3) 0.5020(2) 0.0391(6) Uani 1 d . . .
H32 H 0.4216 0.8755 0.4887 0.047 Uiso 1 calc R . .
C33 C 0.1964(4) 0.9070(3) 0.5656(2) 0.0401(7) Uani 1 d . . .
H33 H 0.2364 0.9577 0.5964 0.048 Uiso 1 calc R . .
C34 C 0.0274(4) 0.8790(3) 0.5833(2) 0.0404(7) Uani 1 d . . .
H34 H -0.0505 0.9102 0.6268 0.049 Uiso 1 calc R . .
C35 C -0.0263(4) 0.8062(3) 0.53763(19) 0.0335(6) Uani 1 d . . .
H35 H -0.1422 0.7874 0.5508 0.040 Uiso 1 calc R . .
C50 C 0.7174(13) 0.4379(8) -0.0649(6) 0.142(3) Uani 1 d . . .
H50A H 0.6120 0.3911 -0.0439 0.170 Uiso 1 calc R . .
H50B H 0.7847 0.4026 -0.1127 0.170 Uiso 1 calc R . .
Cl3 Cl 0.6633(4) 0.5941(2) -0.1031(3) 0.224(2) Uani 1 d . . .
Cl4 Cl 0.8241(7) 0.4087(6) 0.0107(3) 0.261(2) Uani 1 d . . .
C51 C -0.4687(5) 1.0164(4) 0.2454(2) 0.0509(8) Uani 1 d . . .
H51A H -0.5495 0.9562 0.2415 0.061 Uiso 1 calc R . .
H51B H -0.3698 0.9667 0.2635 0.061 Uiso 1 calc R . .
Cl5 Cl -0.40245(15) 1.11431(10) 0.14535(7) 0.0650(3) Uani 1 d . . .
Cl6 Cl -0.56514(14) 1.10486(12) 0.32081(8) 0.0682(3) Uani 1 d . . .
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 0.0000 0.0000 '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_
_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 Ti N3 93.89(9) . . y
N1 Ti N2 94.87(9) . . y
N3 Ti N2 170.64(8) . . y
N1 Ti Cl1 103.05(8) . . y
N3 Ti Cl1 91.80(6) . . y
N2 Ti Cl1 89.44(6) . . y
N1 Ti Cl2 95.39(7) . . y
N3 Ti Cl2 87.68(6) . . y
N2 Ti Cl2 88.21(6) . . y
Cl1 Ti Cl2 161.54(3) . . y
N1 Ti Cl2 172.32(7) . 2_566 ?
N3 Ti Cl2 84.70(6) . 2_566 ?
N2 Ti Cl2 86.18(6) . 2_566 ?
Cl1 Ti Cl2 84.56(2) . 2_566 ?
Cl2 Ti Cl2 77.02(2) . 2_566 ?
Ti Cl2 Ti 102.98(2) . 2_566 y
C1 N1 Ti 165.91(19) . . ?
N1 C1 C6 116.2(2) . . ?
N1 C1 C2 124.3(2) . . ?
C6 C1 C2 119.6(2) . . ?
C3 C2 C1 116.7(3) . . ?
C3 C2 C7 121.1(2) . . ?
C1 C2 C7 122.2(2) . . ?
C4 C3 C2 123.1(3) . . ?
C5 C4 C3 120.0(3) . . ?
C4 C5 C6 119.1(3) . . ?
C5 C6 C1 121.6(3) . . ?
C2 C7 C9 109.6(2) . . ?
C2 C7 C10 110.1(2) . . ?
C9 C7 C10 109.8(2) . . ?
C2 C7 C8 112.2(2) . . ?
C9 C7 C8 108.4(2) . . ?
C10 C7 C8 106.6(3) . . ?
C25 N2 C21 117.2(3) . . ?
C25 N2 Ti 119.45(19) . . ?
C21 N2 Ti 123.24(19) . . ?
N2 C21 C22 123.0(3) . . ?
C23 C22 C21 118.7(3) . . ?
C22 C23 C24 119.1(3) . . ?
C25 C24 C23 118.8(3) . . ?
N2 C25 C24 123.2(3) . . ?
C35 N3 C31 117.3(2) . . ?
C35 N3 Ti 122.74(18) . . ?
C31 N3 Ti 119.92(18) . . ?
N3 C31 C32 122.7(3) . . ?
C31 C32 C33 119.3(3) . . ?
C32 C33 C34 118.1(3) . . ?
C35 C34 C33 119.5(3) . . ?
N3 C35 C34 123.1(3) . . ?
Cl4 C50 Cl3 117.1(6) . . ?
Cl6 C51 Cl5 111.6(2) . . ?
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
Ti N1 1.702(2) . y
Ti N3 2.189(2) . y
Ti N2 2.200(2) . y
Ti Cl1 2.3502(7) . y
Ti Cl2 2.4373(7) . y
Ti Cl2 2.6825(7) 2_566 y
Cl2 Ti 2.6826(7) 2_566 ?
N1 C1 1.379(3) . y
C1 C6 1.383(4) . ?
C1 C2 1.410(3) . ?
C2 C3 1.387(4) . ?
C2 C7 1.518(4) . ?
C3 C4 1.365(5) . ?
C4 C5 1.362(5) . ?
C5 C6 1.382(4) . ?
C7 C9 1.522(4) . ?
C7 C10 1.522(4) . ?
C7 C8 1.526(4) . ?
N2 C25 1.324(4) . ?
N2 C21 1.335(3) . ?
C21 C22 1.365(4) . ?
C22 C23 1.361(5) . ?
C23 C24 1.365(5) . ?
C24 C25 1.364(5) . ?
N3 C35 1.328(4) . ?
N3 C31 1.336(3) . ?
C31 C32 1.364(4) . ?
C32 C33 1.367(5) . ?
C33 C34 1.372(4) . ?
C34 C35 1.353(4) . ?
C50 Cl4 1.620(10) . ?
C50 Cl3 1.705(9) . ?
C51 Cl6 1.732(4) . ?
C51 Cl5 1.740(4) . ?
