#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:43:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179761 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/57/7005705.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_7005705
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         'C28 H44 Cl6 N2 O4 Si4 Zr2, C7 H8'
_chemical_formula_sum            'C35 H52 Cl6 N2 O4 Si4 Zr2'
_chemical_formula_weight         1072.29
_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             2006-05-15T15:56:27-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                102.020(2)
_cell_angle_beta                 97.133(3)
_cell_angle_gamma                109.483(2)
_cell_formula_units_Z            1
_cell_length_a                   8.7913(3)
_cell_length_b                   10.3992(4)
_cell_length_c                   14.8782(7)
_cell_measurement_reflns_used    10909
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     1226.24(9)
_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 0.978
_diffrn_measured_fraction_theta_max 0.978
_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      -0.52561E-2
_diffrn_orient_matrix_UB_12      0.516823E-1
_diffrn_orient_matrix_UB_13      -0.49246E-1
_diffrn_orient_matrix_UB_21      0.12133
_diffrn_orient_matrix_UB_22      0.554613E-1
_diffrn_orient_matrix_UB_23      0.211062E-1
_diffrn_orient_matrix_UB_31      0.219404E-1
_diffrn_orient_matrix_UB_32      -0.738603E-1
_diffrn_orient_matrix_UB_33      -0.45492E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14725
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         3.73
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.885
_exptl_absorpt_correction_T_max  0.8482
_exptl_absorpt_correction_T_min  0.7744
_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    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             546
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.56
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         4708
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0349
_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)+(0.0258P)²+1.4432P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0789
_reflns_number_gt                3836
_reflns_number_total             4708
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b704625a.txt
_cod_data_source_block           (3b)-may1906
_cod_database_code               7005705
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
Zr Zr 0.15145(3) 0.14138(3) 0.12358(2) 0.01875(9) Uani 1 1 d . . .
Cl1 Cl 0.27954(9) 0.07558(8) 0.24809(5) 0.02856(18) Uani 1 1 d . . .
Cl2 Cl 0.37746(9) 0.19968(8) 0.04885(6) 0.03065(19) Uani 1 1 d . . .
Cl3 Cl 0.05335(9) -0.12737(7) 0.02153(5) 0.02493(17) Uani 1 1 d . . .
Si1 Si -0.01856(10) 0.35674(9) 0.20890(6) 0.02267(19) Uani 1 1 d . . .
Si2 Si 0.34623(10) 0.49123(8) 0.20850(6) 0.02106(19) Uani 1 1 d . . .
O1 O -0.0866(2) 0.0650(2) 0.18448(14) 0.0228(5) Uani 1 1 d . . .
O2 O 0.3682(3) 0.6472(2) 0.38922(14) 0.0285(5) Uani 1 1 d . . .
N N 0.1656(3) 0.3379(2) 0.18745(16) 0.0184(5) Uani 1 1 d . . .
C1 C -0.1546(4) -0.1832(3) 0.1944(3) 0.0380(9) Uani 1 1 d . . .
H1A H -0.2322 -0.2493 0.2209 0.057 Uiso 1 1 calc R . .
H1B H -0.0433 -0.1501 0.2331 0.057 Uiso 1 1 calc R . .
H1C H -0.1554 -0.2312 0.1302 0.057 Uiso 1 1 calc R . .
C2 C -0.2045(4) -0.0602(3) 0.1931(2) 0.0270(7) Uani 1 1 d . . .
C3 C -0.3422(4) -0.0367(3) 0.2024(2) 0.0329(8) Uani 1 1 d . . .
H3 H -0.4418 -0.1035 0.209 0.04 Uiso 1 1 calc R . .
C4 C -0.3147(4) 0.1057(3) 0.2010(2) 0.0335(8) Uani 1 1 d . . .
H4 H -0.3938 0.1492 0.206 0.04 Uiso 1 1 calc R . .
C5 C -0.1600(4) 0.1687(3) 0.1915(2) 0.0235(7) Uani 1 1 d . . .
C6 C -0.1029(4) 0.4368(4) 0.1240(2) 0.0349(8) Uani 1 1 d . . .
H6A H -0.1034 0.3883 0.06 0.052 Uiso 1 1 calc R . .
H6B H -0.0338 0.5374 0.1377 0.052 Uiso 1 1 calc R . .
H6C H -0.2158 0.427 0.1296 0.052 Uiso 1 1 calc R . .
C7 C -0.0167(4) 0.4468(4) 0.3307(2) 0.0352(8) Uani 1 1 d . . .
H7A H 0.028 0.4037 0.3748 0.053 Uiso 1 1 calc R . .
H7B H -0.1295 0.437 0.3368 0.053 Uiso 1 1 calc R . .
H7C H 0.0525 0.5475 0.345 0.053 Uiso 1 1 calc R . .
C8 C 0.3660(4) 0.5468(4) 0.0981(2) 0.0354(8) Uani 1 1 d . . .
H8A H 0.3755 0.4711 0.0502 0.053 Uiso 1 1 calc R . .
H8B H 0.4647 0.6327 0.1103 0.053 Uiso 1 1 calc R . .
H8C H 0.2682 0.566 0.0757 0.053 Uiso 1 1 calc R . .
C9 C 0.5288(4) 0.4618(3) 0.2651(2) 0.0311(8) Uani 1 1 d . . .
H9A H 0.5447 0.3835 0.223 0.047 Uiso 1 1 calc R . .
H9B H 0.5104 0.4385 0.3244 0.047 Uiso 1 1 calc R . .
H9C H 0.6274 0.548 0.2777 0.047 Uiso 1 1 calc R . .
C10 C 0.3293(4) 0.6406(3) 0.2943(2) 0.0249(7) Uani 1 1 d . . .
C11 C 0.2840(4) 0.7517(3) 0.2882(2) 0.0301(7) Uani 1 1 d . . .
H11 H 0.2518 0.7741 0.2319 0.036 Uiso 1 1 calc R . .
C12 C 0.2930(4) 0.8285(3) 0.3809(2) 0.0349(8) Uani 1 1 d . . .
H12 H 0.268 0.9112 0.398 0.042 Uiso 1 1 calc R . .
C13 C 0.3439(4) 0.7620(3) 0.4397(2) 0.0323(8) Uani 1 1 d . . .
C14 C 0.3796(5) 0.7876(4) 0.5437(2) 0.0508(10) Uani 1 1 d . . .
H14A H 0.3814 0.8817 0.5735 0.076 Uiso 1 1 calc R . .
H14B H 0.4871 0.7823 0.5644 0.076 Uiso 1 1 calc R . .
H14C H 0.2936 0.7156 0.5618 0.076 Uiso 1 1 calc R . .
C1S C -0.0544(10) 0.0585(10) 0.4333(4) 0.107(3) Uani 1 1 d . . 1
C2S C -0.1586(11) -0.0683(10) 0.4385(4) 0.115(3) Uani 1 1 d . A 1
C3S C -0.1086(11) -0.1351(9) 0.5065(4) 0.111(3) Uani 1 1 d . . 1
C4S C -0.1964(14) -0.2567(13) 0.5098(8) 0.074(3) Uani 0.5 1 d P B 1
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'
Zr Zr -2.9673 0.5597 '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 Zr O1 84.64(8) . . ?
N Zr Cl2 99.82(7) . . ?
O1 Zr Cl2 174.36(5) . . ?
N Zr Cl1 102.59(7) . . ?
O1 Zr Cl1 85.12(5) . . ?
Cl2 Zr Cl1 97.19(3) . . ?
N Zr Cl3 91.61(7) . 2 ?
O1 Zr Cl3 83.72(5) . 2 ?
Cl2 Zr Cl3 92.65(3) . 2 ?
Cl1 Zr Cl3 161.02(3) . 2 ?
N Zr Cl3 165.34(7) . . ?
O1 Zr Cl3 85.91(5) . . ?
Cl2 Zr Cl3 89.03(3) . . ?
Cl1 Zr Cl3 87.72(3) . . ?
Cl3 Zr Cl3 76.22(2) 2 . ?
Zr Cl3 Zr 103.78(2) 2 . ?
N Si1 C7 116.83(14) . . ?
N Si1 C6 112.18(14) . . ?
C7 Si1 C6 110.24(16) . . ?
N Si1 C5 102.44(12) . . ?
C7 Si1 C5 104.20(14) . . ?
C6 Si1 C5 110.23(14) . . ?
N Si2 C10 110.01(13) . . ?
N Si2 C8 109.67(13) . . ?
C10 Si2 C8 106.25(15) . . ?
N Si2 C9 110.26(13) . . ?
C10 Si2 C9 105.35(14) . . ?
C8 Si2 C9 115.08(16) . . ?
C2 O1 C5 107.6(2) . . ?
C2 O1 Zr 140.56(18) . . ?
C5 O1 Zr 108.98(16) . . ?
C13 O2 C10 107.8(2) . . ?
Si1 N Si2 119.27(13) . . ?
Si1 N Zr 117.01(12) . . ?
Si2 N Zr 123.23(13) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 O1 108.0(3) . . ?
C3 C2 C1 133.5(3) . . ?
O1 C2 C1 118.4(3) . . ?
C2 C3 C4 108.3(3) . . ?
C2 C3 H3 125.8 . . ?
C4 C3 H3 125.8 . . ?
C5 C4 C3 109.3(3) . . ?
C5 C4 H4 125.3 . . ?
C3 C4 H4 125.3 . . ?
C4 C5 O1 106.7(3) . . ?
C4 C5 Si1 135.0(3) . . ?
O1 C5 Si1 116.96(19) . . ?
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 . . ?
Si1 C7 H7A 109.5 . . ?
Si1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si1 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 . . ?
Si2 C9 H9A 109.5 . . ?
Si2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 O2 107.6(3) . . ?
C11 C10 Si2 135.1(2) . . ?
O2 C10 Si2 117.2(2) . . ?
C10 C11 C12 107.9(3) . . ?
C10 C11 H11 126 . . ?
C12 C11 H11 126 . . ?
C13 C12 C11 107.0(3) . . ?
C13 C12 H12 126.5 . . ?
C11 C12 H12 126.5 . . ?
C12 C13 O2 109.6(3) . . ?
C12 C13 C14 134.3(3) . . ?
O2 C13 C14 116.0(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C2S C1S C3S 123.9(7) . 2_556 ?
C1S C2S C3S 119.8(8) . . ?
C4S C3S C2S 122.0(10) . . ?
C4S C3S C1S 121.5(8) . 2_556 ?
C2S C3S C1S 116.3(8) . 2_556 ?
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
Zr N 2.021(2) . ?
Zr O1 2.3438(19) . ?
Zr Cl2 2.3616(8) . ?
Zr Cl1 2.3859(8) . ?
Zr Cl3 2.5793(7) 2 ?
Zr Cl3 2.6757(8) . ?
Cl3 Zr 2.5793(7) 2 ?
Si1 N 1.754(2) . ?
Si1 C7 1.855(3) . ?
Si1 C6 1.859(3) . ?
Si1 C5 1.878(3) . ?
Si2 N 1.773(2) . ?
Si2 C10 1.855(3) . ?
Si2 C8 1.860(3) . ?
Si2 C9 1.865(3) . ?
O1 C2 1.410(3) . ?
O1 C5 1.422(3) . ?
O2 C13 1.368(4) . ?
O2 C10 1.393(3) . ?
C1 C2 1.487(4) . ?
C1 H1A 0.98 . ?
C1 H1B 0.98 . ?
C1 H1C 0.98 . ?
C2 C3 1.330(4) . ?
C3 C4 1.423(5) . ?
C3 H3 0.95 . ?
C4 C5 1.338(4) . ?
C4 H4 0.95 . ?
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 H9A 0.98 . ?
C9 H9B 0.98 . ?
C9 H9C 0.98 . ?
C10 C11 1.358(4) . ?
C11 C12 1.421(5) . ?
C11 H11 0.95 . ?
C12 C13 1.345(5) . ?
C12 H12 0.95 . ?
C13 C14 1.488(5) . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
C1S C2S 1.356(10) . ?
C1S C3S 1.454(10) 2_556 ?
C2S C3S 1.443(9) . ?
C3S C4S 1.258(12) . ?
C3S C1S 1.454(10) 2_556 ?
