#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:35:12 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179797 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/93/7009376.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_7009376
loop_
_publ_author_name
'Fernández-Galán, Rafael'
'Hitchcock, Peter B.'
'Lappert, Michael F.'
'Antiñolo, Antonio'
'Rodríguez, Ana M.'
_publ_section_title
;
 Synthesis and structural characterisation of new ansa-bis(propene)s
 and {ansa-bis(allyl)}alkali metal and {ansa-bis(allyl)}transition
 metal complexes
;
_journal_issue                   11
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1743
_journal_paper_doi               10.1039/b000451k
_journal_year                    2000
_chemical_formula_structural     '[Zr{Me3Si(CH)3SiMe2(CH)3SiMe3)}2]'
_chemical_formula_sum            'C28 H60 Si6 Zr'
_chemical_formula_weight         656.52
_chemical_name_systematic
; 
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 103.39(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.512(2)
_cell_length_b                   17.267(3)
_cell_length_c                   19.367(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     3745.1(10)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_molecular_graphics    'CAMERON (Watkin and Pearce,1993)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       ' Enraf-Nonius CAD4'
_diffrn_measurement_method       ω--2θ
_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  0.0452
_diffrn_reflns_av_sigmaI/netI    0.1037
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            4830
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.501
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.043
_refine_ls_goodness_of_fit_obs   1.096
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         4622
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_restrained_S_obs      1.096
_refine_ls_R_factor_all          0.1216
_refine_ls_R_factor_obs          0.0627
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0650P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1661
_refine_ls_wR_factor_obs         0.1357
_reflns_number_observed          2835
_reflns_number_total             4622
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b000451k.txt
_cod_data_source_block           may898
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+0.0000P] 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^)+(0.0650P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7009376
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y, -z-1/2'
'-x+1/2, -y+1/2, -z'
'-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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Zr Zr 0.0000 0.17604(4) 0.2500 0.0312(2) Uani 1 d S .
Si1 Si 0.16607(14) 0.05666(9) 0.11641(8) 0.0515(4) Uani 1 d . .
Si2 Si -0.23226(13) 0.16099(9) 0.12958(8) 0.0502(4) Uani 1 d . .
Si3 Si -0.17613(15) 0.32434(10) 0.34868(8) 0.0556(4) Uani 1 d . .
C1 C 0.0353(4) 0.1020(3) 0.1401(3) 0.0405(11) Uani 1 d . .
H1 H 0.0049(40) 0.1402(27) 0.1157(23) 0.034(13) Uiso 1 d . .
C2 C -0.0426(5) 0.0598(3) 0.1698(3) 0.0409(11) Uani 1 d . .
H2 H -0.0190(38) 0.0174(26) 0.1847(22) 0.029(12) Uiso 1 d . .
C3 C -0.1488(5) 0.0843(3) 0.1841(3) 0.0440(12) Uani 1 d . .
H3 H -0.1740(45) 0.0538(29) 0.2099(26) 0.047(16) Uiso 1 d . .
C4 C -0.1379(5) 0.2477(3) 0.1532(3) 0.0458(12) Uani 1 d . .
H4 H -0.1016(56) 0.2717(37) 0.1247(34) 0.091(23) Uiso 1 d . .
C5 C -0.1383(5) 0.2896(3) 0.2123(3) 0.0457(12) Uani 1 d . .
H5 H -0.1111(44) 0.3412(29) 0.2127(26) 0.048(15) Uiso 1 d . .
C6 C -0.1564(5) 0.2612(3) 0.2757(3) 0.0454(12) Uani 1 d . .
H6 H -0.2034(42) 0.2191(28) 0.2655(25) 0.046(14) Uiso 1 d . .
C7 C 0.1702(6) -0.0473(3) 0.1392(3) 0.071(2) Uani 1 d . .
H7C H 0.2382(6) -0.0710(3) 0.1269(3) 0.107 Uiso 1 calc R .
H7B H 0.0985(6) -0.0718(3) 0.1133(3) 0.107 Uiso 1 calc R .
H7A H 0.1762(6) -0.0530(3) 0.1892(3) 0.107 Uiso 1 calc R .
C8 C 0.1492(6) 0.0660(4) 0.0190(3) 0.075(2) Uani 1 d . .
H8C H 0.1469(6) 0.1198(4) 0.0063(3) 0.113 Uiso 1 calc R .
H8B H 0.0763(6) 0.0414(4) -0.0053(3) 0.113 Uiso 1 calc R .
H8A H 0.2156(6) 0.0415(4) 0.0056(3) 0.113 Uiso 1 calc R .
C9 C 0.3145(5) 0.0965(4) 0.1601(4) 0.088(2) Uani 1 d . .
H9C H 0.3167(5) 0.1508(4) 0.1498(4) 0.132 Uiso 1 calc R .
H9B H 0.3753(5) 0.0701(4) 0.1427(4) 0.132 Uiso 1 calc R .
H9A H 0.3282(5) 0.0893(4) 0.2105(4) 0.132 Uiso 1 calc R .
C10 C -0.3850(5) 0.1734(4) 0.1457(4) 0.083(2) Uani 1 d . .
H10C H -0.4258(5) 0.2142(4) 0.1160(4) 0.125 Uiso 1 calc R .
H10B H -0.3787(5) 0.1864(4) 0.1946(4) 0.125 Uiso 1 calc R .
H10A H -0.4290(5) 0.1260(4) 0.1347(4) 0.125 Uiso 1 calc R .
C11 C -0.2501(6) 0.1399(4) 0.0330(3) 0.075(2) Uani 1 d . .
H11C H -0.2943(6) 0.1810(4) 0.0054(3) 0.113 Uiso 1 calc R .
H11B H -0.2925(6) 0.0919(4) 0.0215(3) 0.113 Uiso 1 calc R .
H11A H -0.1729(6) 0.1358(4) 0.0225(3) 0.113 Uiso 1 calc R .
C12 C -0.1268(6) 0.2814(4) 0.4383(3) 0.073(2) Uani 1 d . .
H12C H -0.1688(6) 0.2338(4) 0.4404(3) 0.109 Uiso 1 calc R .
H12B H -0.1433(6) 0.3169(4) 0.4730(3) 0.109 Uiso 1 calc R .
H12A H -0.0425(6) 0.2714(4) 0.4481(3) 0.109 Uiso 1 calc R .
C13 C -0.3389(6) 0.3463(4) 0.3342(4) 0.080(2) Uani 1 d . .
H13C H -0.3824(6) 0.2990(4) 0.3347(4) 0.120 Uiso 1 calc R .
H13B H -0.3661(6) 0.3715(4) 0.2892(4) 0.120 Uiso 1 calc R .
H13A H -0.3518(6) 0.3797(4) 0.3714(4) 0.120 Uiso 1 calc R .
C14 C -0.0930(7) 0.4151(4) 0.3478(4) 0.083(2) Uani 1 d . .
H14C H -0.1037(7) 0.4477(4) 0.3860(4) 0.125 Uiso 1 calc R .
H14B H -0.1222(7) 0.4411(4) 0.3034(4) 0.125 Uiso 1 calc R .
H14A H -0.0097(7) 0.4037(4) 0.3535(4) 0.125 Uiso 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 0.0000 0.0000 '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
C3 Zr C3 99.9(3) . 6_556 ?
C3 Zr C6 137.1(2) . 6_556 ?
C3 Zr C6 92.0(2) 6_556 6_556 ?
C3 Zr C6 92.0(2) . . ?
C3 Zr C6 137.1(2) 6_556 . ?
C6 Zr C6 106.7(3) 6_556 . ?
C3 Zr C4 163.1(2) . 6_556 ?
C3 Zr C4 71.5(2) 6_556 6_556 ?
C6 Zr C4 59.1(2) 6_556 6_556 ?
C6 Zr C4 85.4(2) . 6_556 ?
C3 Zr C4 71.5(2) . . ?
C3 Zr C4 163.1(2) 6_556 . ?
C6 Zr C4 85.4(2) 6_556 . ?
C6 Zr C4 59.1(2) . . ?
C4 Zr C4 120.3(3) 6_556 . ?
C3 Zr C2 32.2(2) . . ?
C3 Zr C2 79.6(2) 6_556 . ?
C6 Zr C2 113.5(2) 6_556 . ?
C6 Zr C2 123.6(2) . . ?
C4 Zr C2 149.5(2) 6_556 . ?
C4 Zr C2 86.1(2) . . ?
C3 Zr C2 79.6(2) . 6_556 ?
C3 Zr C2 32.2(2) 6_556 6_556 ?
C6 Zr C2 123.6(2) 6_556 6_556 ?
C6 Zr C2 113.5(2) . 6_556 ?
C4 Zr C2 86.1(2) 6_556 6_556 ?
C4 Zr C2 149.5(2) . 6_556 ?
C2 Zr C2 74.1(2) . 6_556 ?
C3 Zr C5 165.0(2) . 6_556 ?
C3 Zr C5 91.9(2) 6_556 6_556 ?
C6 Zr C5 32.1(2) 6_556 6_556 ?
C6 Zr C5 85.4(2) . 6_556 ?
C4 Zr C5 31.4(2) 6_556 6_556 ?
C4 Zr C5 94.6(2) . 6_556 ?
C2 Zr C5 144.9(2) . 6_556 ?
C2 Zr C5 114.9(2) 6_556 6_556 ?
C3 Zr C5 91.9(2) . . ?
C3 Zr C5 165.0(2) 6_556 . ?
C6 Zr C5 85.4(2) 6_556 . ?
C6 Zr C5 32.1(2) . . ?
C4 Zr C5 94.6(2) 6_556 . ?
C4 Zr C5 31.4(2) . . ?
C2 Zr C5 114.9(2) . . ?
C2 Zr C5 144.9(2) 6_556 . ?
C5 Zr C5 78.1(3) 6_556 . ?
C3 Zr C1 58.7(2) . . ?
C3 Zr C1 83.5(2) 6_556 . ?
C6 Zr C1 82.4(2) 6_556 . ?
C6 Zr C1 136.1(2) . . ?
C4 Zr C1 132.0(2) 6_556 . ?
C4 Zr C1 79.7(2) . . ?
C2 Zr C1 31.3(2) . . ?
C2 Zr C1 93.9(2) 6_556 . ?
C5 Zr C1 114.3(2) 6_556 . ?
C5 Zr C1 110.7(2) . . ?
C3 Zr C1 83.5(2) . 6_556 ?
C3 Zr C1 58.7(2) 6_556 6_556 ?
C6 Zr C1 136.1(2) 6_556 6_556 ?
C6 Zr C1 82.4(2) . 6_556 ?
C4 Zr C1 79.7(2) 6_556 6_556 ?
C4 Zr C1 132.0(2) . 6_556 ?
C2 Zr C1 93.9(2) . 6_556 ?
C2 Zr C1 31.3(2) 6_556 6_556 ?
C5 Zr C1 110.7(2) 6_556 6_556 ?
C5 Zr C1 114.3(2) . 6_556 ?
C1 Zr C1 120.9(2) . 6_556 ?
C7 Si1 C1 109.3(3) . . ?
C7 Si1 C9 106.3(3) . . ?
C1 Si1 C9 116.6(3) . . ?
C7 Si1 C8 108.5(3) . . ?
C1 Si1 C8 108.4(3) . . ?
C9 Si1 C8 107.5(3) . . ?
C3 Si2 C4 104.2(2) . . ?
C3 Si2 C10 112.2(3) . . ?
C4 Si2 C10 112.8(3) . . ?
C3 Si2 C11 111.0(3) . . ?
C4 Si2 C11 109.2(3) . . ?
C10 Si2 C11 107.4(3) . . ?
C3 Si2 Zr 51.9(2) . . ?
C4 Si2 Zr 52.7(2) . . ?
C10 Si2 Zr 122.8(2) . . ?
C11 Si2 Zr 129.8(2) . . ?
C14 Si3 C6 109.9(3) . . ?
C14 Si3 C12 107.6(3) . . ?
C6 Si3 C12 114.7(3) . . ?
C14 Si3 C13 109.4(3) . . ?
C6 Si3 C13 107.7(3) . . ?
C12 Si3 C13 107.5(3) . . ?
C2 C1 Si1 121.7(4) . . ?
C2 C1 Zr 71.2(3) . . ?
Si1 C1 Zr 134.8(2) . . ?
C3 C2 C1 127.7(5) . . ?
C3 C2 Zr 71.8(3) . . ?
C1 C2 Zr 77.5(3) . . ?
C2 C3 Si2 118.7(4) . . ?
C2 C3 Zr 76.1(3) . . ?
Si2 C3 Zr 92.5(2) . . ?
C5 C4 Si2 121.7(5) . . ?
C5 C4 Zr 75.8(3) . . ?
Si2 C4 Zr 91.1(2) . . ?
C4 C5 C6 126.2(6) . . ?
C4 C5 Zr 72.8(3) . . ?
C6 C5 Zr 71.4(3) . . ?
C5 C6 Si3 122.8(4) . . ?
C5 C6 Zr 76.4(3) . . ?
Si3 C6 Zr 137.3(3) . . ?
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 C3 2.462(5) . ?
Zr C3 2.462(5) 6_556 ?
Zr C6 2.462(5) 6_556 ?
Zr C6 2.462(5) . ?
Zr C4 2.488(5) 6_556 ?
Zr C4 2.488(5) . ?
Zr C2 2.516(5) . ?
Zr C2 2.516(5) 6_556 ?
Zr C5 2.525(5) 6_556 ?
Zr C5 2.525(5) . ?
Zr C1 2.594(5) . ?
Zr C1 2.594(5) 6_556 ?
Si1 C7 1.846(6) . ?
Si1 C1 1.846(5) . ?
Si1 C9 1.854(6) . ?
Si1 C8 1.859(6) . ?
Si2 C3 1.822(6) . ?
Si2 C4 1.844(6) . ?
Si2 C10 1.868(6) . ?
Si2 C11 1.870(6) . ?
Si3 C14 1.838(7) . ?
Si3 C6 1.841(5) . ?
Si3 C12 1.852(6) . ?
Si3 C13 1.868(6) . ?
C1 C2 1.381(7) . ?
C2 C3 1.381(7) . ?
C4 C5 1.355(7) . ?
C5 C6 1.382(7) . ?
