#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/00/57/7005702.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_7005702
loop_
_publ_author_name
'Evans, Lloyd T. J.'
'Coles, Martyn P.'
'Geoffrey, F.'
'Cloke, N.'
'Hitchcock, Peter B.'
_publ_section_title
;
 Deactivation pathways of ethylene polymerization catalysts derived
 from titanium and zirconium
 1,3-bis(furyl)-1,1,3,3-tetramethyldisilazide complexes.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2707
_journal_page_last               2717
_journal_paper_doi               10.1039/b704625a
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C12 H18 Cl3 N O2 Si2 Ti'
_chemical_formula_sum            'C12 H18 Cl3 N O2 Si2 Ti'
_chemical_formula_weight         418.7
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2006-04-06T16:15:45-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                97.848(2)
_cell_angle_beta                 90.932(2)
_cell_angle_gamma                96.928(2)
_cell_formula_units_Z            2
_cell_length_a                   6.8208(2)
_cell_length_b                   9.3822(3)
_cell_length_c                   15.0516(6)
_cell_measurement_reflns_used    9672
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     946.70(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.146541
_diffrn_orient_matrix_UB_12      0.270447E-1
_diffrn_orient_matrix_UB_13      0.4599E-2
_diffrn_orient_matrix_UB_21      -0.37628E-2
_diffrn_orient_matrix_UB_22      0.55456E-2
_diffrn_orient_matrix_UB_23      0.667613E-1
_diffrn_orient_matrix_UB_31      0.186458E-1
_diffrn_orient_matrix_UB_32      -0.104856
_diffrn_orient_matrix_UB_33      -0.49665E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13530
_diffrn_reflns_theta_full        25.96
_diffrn_reflns_theta_max         25.96
_diffrn_reflns_theta_min         3.69
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.003
_exptl_absorpt_correction_T_max  0.7905
_exptl_absorpt_correction_T_min  0.7198
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.34
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         3688
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0848
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0736P)²+16.7351P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2494
_refine_ls_wR_factor_ref         0.2547
_reflns_number_gt                3295
_reflns_number_total             3688
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b704625a.txt
_cod_data_source_block           (1a)-apr806
_cod_database_code               7005702
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti Ti 0.3381(2) 0.89373(15) 0.25690(10) 0.0257(4) Uani 1 1 d . . .
Cl1 Cl 0.6476(3) 0.8577(3) 0.22768(18) 0.0434(6) Uani 1 1 d . . .
Cl2 Cl 0.2107(4) 1.0547(2) 0.18436(16) 0.0421(6) Uani 1 1 d . . .
Cl3 Cl 0.3688(4) 1.0142(3) 0.39347(16) 0.0463(6) Uani 1 1 d . . .
Si1 Si 0.1135(3) 0.6614(2) 0.37194(14) 0.0239(5) Uani 1 1 d . . .
Si2 Si 0.1562(3) 0.6070(2) 0.16309(14) 0.0228(5) Uani 1 1 d . . .
O1 O -0.2310(9) 0.4648(7) 0.3318(4) 0.0350(14) Uani 1 1 d . . .
O2 O 0.0811(11) 0.7845(8) 0.0370(4) 0.0424(16) Uani 1 1 d . . .
N N 0.1859(10) 0.7225(7) 0.2677(4) 0.0232(13) Uani 1 1 d . . .
C1 C -0.2946(16) 0.3200(11) 0.3162(7) 0.044(2) Uani 1 1 d . . .
H1 H -0.4285 0.2809 0.3029 0.052 Uiso 1 1 calc R . .
C2 C -0.1504(16) 0.2406(10) 0.3215(7) 0.045(2) Uani 1 1 d . . .
H2 H -0.1603 0.1377 0.3134 0.053 Uiso 1 1 calc R . .
C3 C 0.0264(15) 0.3416(10) 0.3421(6) 0.036(2) Uani 1 1 d . . .
H3 H 0.1563 0.3179 0.3507 0.044 Uiso 1 1 calc R . .
C4 C -0.0284(12) 0.4775(9) 0.3469(5) 0.0273(17) Uani 1 1 d . . .
C5 C 0.3397(14) 0.6400(11) 0.4370(6) 0.037(2) Uani 1 1 d . . .
H5A H 0.4199 0.7345 0.4519 0.056 Uiso 1 1 calc R . .
H5B H 0.4165 0.5729 0.4009 0.056 Uiso 1 1 calc R . .
H5C H 0.3019 0.6013 0.4924 0.056 Uiso 1 1 calc R . .
C6 C -0.0550(14) 0.7817(10) 0.4306(6) 0.036(2) Uani 1 1 d . . .
H6A H 0.0144 0.8802 0.445 0.055 Uiso 1 1 calc R . .
H6B H -0.0972 0.7452 0.4861 0.055 Uiso 1 1 calc R . .
H6C H -0.171 0.7833 0.3916 0.055 Uiso 1 1 calc R . .
C7 C -0.1019(14) 0.5322(11) 0.1349(6) 0.039(2) Uani 1 1 d . . .
H7A H -0.1837 0.6116 0.1373 0.058 Uiso 1 1 calc R . .
H7B H -0.1486 0.4674 0.178 0.058 Uiso 1 1 calc R . .
H7C H -0.1111 0.4778 0.0743 0.058 Uiso 1 1 calc R . .
C8 C 0.3269(14) 0.4678(10) 0.1600(7) 0.037(2) Uani 1 1 d . . .
H8A H 0.4617 0.515 0.1751 0.055 Uiso 1 1 calc R . .
H8B H 0.3224 0.4125 0.0997 0.055 Uiso 1 1 calc R . .
H8C H 0.2871 0.4021 0.2036 0.055 Uiso 1 1 calc R . .
C9 C 0.2335(13) 0.7279(9) 0.0780(5) 0.0284(17) Uani 1 1 d . . .
C10 C 0.4010(15) 0.7568(9) 0.0332(6) 0.035(2) Uani 1 1 d . . .
H10 H 0.526 0.7278 0.0461 0.042 Uiso 1 1 calc R . .
C11 C 0.358(2) 0.8385(12) -0.0366(6) 0.054(3) Uani 1 1 d . . .
H11 H 0.4463 0.8743 -0.0788 0.064 Uiso 1 1 calc R . .
C12 C 0.165(2) 0.8537(12) -0.0298(7) 0.052(3) Uani 1 1 d . . .
H12 H 0.0958 0.9063 -0.0669 0.062 Uiso 1 1 calc R . .
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'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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
N Ti Cl3 105.2(2) . . ?
N Ti Cl1 111.0(2) . . ?
Cl3 Ti Cl1 102.19(12) . . ?
N Ti Cl2 118.8(2) . . ?
Cl3 Ti Cl2 100.12(11) . . ?
Cl1 Ti Cl2 116.60(12) . . ?
N Si1 C6 110.3(4) . . ?
N Si1 C5 108.7(4) . . ?
C6 Si1 C5 115.8(4) . . ?
N Si1 C4 108.6(3) . . ?
C6 Si1 C4 106.9(4) . . ?
C5 Si1 C4 106.3(4) . . ?
N Si2 C7 113.0(4) . . ?
N Si2 C8 109.8(4) . . ?
C7 Si2 C8 113.7(5) . . ?
N Si2 C9 104.7(3) . . ?
C7 Si2 C9 106.7(4) . . ?
C8 Si2 C9 108.3(4) . . ?
C1 O1 C4 106.3(7) . . ?
C12 O2 C9 106.1(8) . . ?
Si2 N Si1 122.7(4) . . ?
Si2 N Ti 111.1(3) . . ?
Si1 N Ti 125.3(4) . . ?
C2 C1 O1 112.5(9) . . ?
C2 C1 H1 123.7 . . ?
O1 C1 H1 123.7 . . ?
C1 C2 C3 105.8(8) . . ?
C1 C2 H2 127.1 . . ?
C3 C2 H2 127.1 . . ?
C4 C3 C2 107.0(9) . . ?
C4 C3 H3 126.5 . . ?
C2 C3 H3 126.5 . . ?
C3 C4 O1 108.4(8) . . ?
C3 C4 Si1 132.4(7) . . ?
O1 C4 Si1 119.2(6) . . ?
Si1 C5 H5A 109.5 . . ?
Si1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si2 C8 H8A 109.5 . . ?
Si2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 O2 108.4(8) . . ?
C10 C9 Si2 134.8(7) . . ?
O2 C9 Si2 115.6(6) . . ?
C9 C10 C11 108.3(10) . . ?
C9 C10 H10 125.8 . . ?
C11 C10 H10 125.8 . . ?
C12 C11 C10 105.2(9) . . ?
C12 C11 H11 127.4 . . ?
C10 C11 H11 127.4 . . ?
C11 C12 O2 111.8(9) . . ?
C11 C12 H12 124.1 . . ?
O2 C12 H12 124.1 . . ?
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 N 1.833(6) . ?
Ti Cl3 2.200(3) . ?
Ti Cl1 2.219(3) . ?
Ti Cl2 2.228(3) . ?
Si1 N 1.799(7) . ?
Si1 C6 1.857(9) . ?
Si1 C5 1.860(9) . ?
Si1 C4 1.861(9) . ?
Si2 N 1.779(6) . ?
Si2 C7 1.835(9) . ?
Si2 C8 1.848(9) . ?
Si2 C9 1.866(9) . ?
O1 C1 1.362(11) . ?
O1 C4 1.385(10) . ?
O2 C12 1.367(13) . ?
O2 C9 1.395(10) . ?
C1 C2 1.311(15) . ?
C1 H1 0.95 . ?
C2 C3 1.442(13) . ?
C2 H2 0.95 . ?
C3 C4 1.365(12) . ?
C3 H3 0.95 . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
C8 H8A 0.98 . ?
C8 H8B 0.98 . ?
C8 H8C 0.98 . ?
C9 C10 1.354(13) . ?
C10 C11 1.430(14) . ?
C10 H10 0.95 . ?
C11 C12 1.342(18) . ?
C11 H11 0.95 . ?
C12 H12 0.95 . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30652692
