#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:26:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179844 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/40/7014044.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_7014044
loop_
_publ_author_name
'Möller, Andreas C'
'Heyn, Richard H.'
'Blom, Richard'
'Swang, Ole'
'Görbitz, Carl Henrik'
'Kopf, Jürgen'
_publ_section_title
;
 Synthesis, structure, and ethene polymerisation catalysis of 1- or
 2-silyl substituted bis[indenyl]zirconium(IV) dichlorides.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1578
_journal_page_last               1589
_journal_paper_doi               10.1039/b400505h
_journal_year                    2004
_chemical_absolute_configuration racemate
_chemical_compound_source        synthesis
_chemical_formula_sum            'C22 H26 Cl2 Si2 Zr'
_chemical_formula_weight         508.73
_chemical_name_common            Zr-metallorganic
_chemical_name_systematic
;
Zr-metallorganic
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.783(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6354(1)
_cell_length_b                   13.4550(2)
_cell_length_c                   16.3064(1)
_cell_measurement_reflns_used    7490
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      45.0
_cell_measurement_theta_min      2.9
_cell_volume                     2306.07(4)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXTL (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device       'Siemens SMART CCD diffractometer'
_diffrn_measurement_method
'Sets of exposures each taken over 0.6° ω rotation'
_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  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0441
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            44638
_diffrn_reflns_theta_full        35.00
_diffrn_reflns_theta_max         45.01
_diffrn_reflns_theta_min         2.90
_diffrn_standards_decay_%        0
_diffrn_standards_number         'not applicable to area detectors'
_exptl_absorpt_coefficient_mu    0.818
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.214
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         18142
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0394P)²+0.2286P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0917
_reflns_number_gt                12448
_reflns_number_total             18142
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b400505h.txt
_cod_data_source_block           rh
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7014044
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.076673(9) 0.620267(7) 0.196682(6) 0.01319(2) Uani 1 d . .
Cl1 Cl 0.22022(3) 0.49884(2) 0.14812(2) 0.02296(5) Uani 1 d . .
Cl2 Cl -0.08929(3) 0.50047(2) 0.21499(2) 0.02230(5) Uani 1 d . .
Si1A Si -0.27826(3) 0.68630(3) 0.11630(2) 0.02150(6) Uani 1 d . .
H1A H -0.28453 0.68288 0.17681 0.026 Uiso 1 calc R .
Si1B Si 0.43052(3) 0.67585(3) 0.27279(2) 0.02056(6) Uani 1 d . .
H1B H 0.42557 0.67376 0.21108 0.025 Uiso 1 calc R .
C1A C 0.08310(10) 0.68836(9) 0.04792(6) 0.0182(2) Uani 1 d . .
C2A C 0.09090(10) 0.77284(8) 0.10190(7) 0.0171(2) Uani 1 d . .
C3A C -0.02484(10) 0.77620(8) 0.13700(6) 0.01633(15) Uani 1 d . .
H3A H -0.05158 0.83276 0.17020 0.020 Uiso 1 calc R .
C4A C -0.10645(10) 0.69753(8) 0.10231(7) 0.0168(2) Uani 1 d . .
C5A C -0.03697(11) 0.64034(9) 0.05087(7) 0.0185(2) Uani 1 d . .
H5A H -0.07285 0.58470 0.01385 0.022 Uiso 1 calc R .
C6A C 0.19764(11) 0.83877(9) 0.10845(8) 0.0227(2) Uani 1 d . .
H6A H 0.20425 0.89416 0.14499 0.027 Uiso 1 calc R .
C7A C 0.29000(12) 0.81961(12) 0.06046(9) 0.0286(3) Uani 1 d . .
H7A H 0.35957 0.86424 0.06216 0.034 Uiso 1 calc R .
C8A C 0.28430(13) 0.73425(12) 0.00796(9) 0.0292(3) Uani 1 d . .
H8A H 0.35121 0.72255 -0.02333 0.035 Uiso 1 calc R .
C9A C 0.18413(12) 0.66859(11) 0.00168(8) 0.0247(2) Uani 1 d . .
H9A H 0.18217 0.61139 -0.03264 0.030 Uiso 1 calc R .
C10A C -0.35869(14) 0.57664(12) 0.06230(11) 0.0340(3) Uani 1 d . .
H10A H -0.3245 0.5198 0.0868 0.051 Uiso 1 calc R .
H11A H -0.3476 0.5774 0.0079 0.051 Uiso 1 calc R .
H12A H -0.4435 0.5789 0.0657 0.051 Uiso 1 calc R .
C11A C -0.3541(2) 0.80438(14) 0.0712(2) 0.0478(5) Uani 1 d . .
H13A H -0.3012 0.8606 0.0915 0.072 Uiso 1 calc R .
H14A H -0.4376 0.8117 0.0877 0.072 Uiso 1 calc R .
H15A H -0.3628 0.8017 0.0111 0.072 Uiso 1 calc R .
C1B C 0.09158(10) 0.61170(8) 0.36000(6) 0.0170(2) Uani 1 d . .
C2B C 0.06565(10) 0.71212(8) 0.33198(6) 0.01604(15) Uani 1 d . .
C3B C 0.17323(10) 0.74597(8) 0.29604(6) 0.01631(15) Uani 1 d . .
H3B H 0.18963 0.81664 0.28192 0.020 Uiso 1 calc R .
C4B C 0.26508(10) 0.66740(8) 0.30101(7) 0.0171(2) Uani 1 d . .
C5B C 0.21133(11) 0.58369(8) 0.33729(7) 0.0180(2) Uani 1 d . .
H5B H 0.25663 0.51971 0.35284 0.022 Uiso 1 calc R .
C6B C -0.05065(11) 0.75941(9) 0.34427(7) 0.0200(2) Uani 1 d . .
H6B H -0.07021 0.82482 0.32438 0.024 Uiso 1 calc R .
C7B C -0.13313(12) 0.70786(11) 0.38551(8) 0.0241(2) Uani 1 d . .
H7B H -0.21029 0.73852 0.39456 0.029 Uiso 1 calc R .
C8B C -0.10556(12) 0.60905(10) 0.41518(7) 0.0243(2) Uani 1 d . .
H8B H -0.16414 0.57618 0.44445 0.029 Uiso 1 calc R .
C9B C 0.00333(12) 0.56039(9) 0.40248(7) 0.0215(2) Uani 1 d . .
H9B H 0.01950 0.49421 0.42151 0.026 Uiso 1 calc R .
C10B C 0.52424(15) 0.56733(13) 0.31998(13) 0.0375(3) Uani 1 d . .
H10B H 0.4851 0.5085 0.2992 0.056 Uiso 1 calc R .
H11B H 0.5280 0.5690 0.3775 0.056 Uiso 1 calc R .
H12B H 0.6066 0.5702 0.3068 0.056 Uiso 1 calc R .
C11B C 0.4998(2) 0.79716(12) 0.31305(13) 0.0369(3) Uani 1 d . .
H13B H 0.4472 0.8475 0.2924 0.055 Uiso 1 calc R .
H14B H 0.5773 0.8056 0.2969 0.055 Uiso 1 calc R .
H15B H 0.5086 0.7975 0.3694 0.055 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'
Cl Cl 0.1484 0.1585 '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
Cl2 Zr Cl1 95.572(11) . . ?
C10A Si1A C11A 110.26(9) . . ?
C10A Si1A C4A 113.05(6) . . ?
C11A Si1A C4A 104.56(7) . . ?
C4A Si1A H1A 109.6 . . ?
C10B Si1B C11B 112.43(9) . . ?
C10B Si1B C4B 108.13(6) . . ?
C11B Si1B C4B 107.41(6) . . ?
C4B Si1B H1B 109.6 . . ?
C9A C1A C2A 119.63(11) . . ?
C9A C1A C5A 132.61(11) . . ?
C2A C1A C5A 107.73(9) . . ?
C6A C2A C1A 120.57(10) . . ?
C6A C2A C3A 132.00(11) . . ?
C1A C2A C3A 107.30(9) . . ?
C4A C3A C2A 108.94(9) . . ?
C5A C4A C3A 107.14(9) . . ?
C5A C4A Si1A 128.93(8) . . ?
C3A C4A Si1A 123.61(8) . . ?
C4A C5A C1A 108.65(10) . . ?
C7A C6A C2A 118.04(13) . . ?
C6A C7A C8A 121.67(12) . . ?
C9A C8A C7A 121.50(12) . . ?
C8A C9A C1A 118.52(13) . . ?
C9B C1B C5B 132.53(10) . . ?
C9B C1B C2B 120.00(10) . . ?
C5B C1B C2B 107.47(9) . . ?
C6B C2B C3B 132.44(10) . . ?
C6B C2B C1B 120.02(10) . . ?
C3B C2B C1B 107.52(9) . . ?
C4B C3B C2B 108.75(9) . . ?
C5B C4B C3B 106.98(9) . . ?
C5B C4B Si1B 126.42(8) . . ?
C3B C4B Si1B 126.44(8) . . ?
C1B C5B C4B 109.10(9) . . ?
C7B C6B C2B 118.32(11) . . ?
C6B C7B C8B 121.50(11) . . ?
C9B C8B C7B 121.76(11) . . ?
C8B C9B C1B 118.35(11) . . ?
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 Cl2 2.4421(3) . ?
Zr Cl1 2.4487(3) . ?
Zr C1A 2.6036(10) . ?
Zr C1B 2.6461(10) . ?
Zr C2A 2.5880(10) . ?
Zr C2B 2.5470(10) . ?
Zr C3A 2.4888(10) . ?
Zr C3B 2.4560(10) . ?
Zr C4A 2.5153(10) . ?
Zr C4B 2.5041(11) . ?
Zr C5A 2.5119(11) . ?
Zr C5B 2.5589(11) . ?
Si1A C10A 1.8586(15) . ?
Si1A C11A 1.880(2) . ?
Si1A C4A 1.8818(11) . ?
Si1A H1A 1.00 . ?
Si1B C10B 1.866(2) . ?
Si1B C11B 1.868(2) . ?
Si1B C4B 1.8889(11) . ?
Si1B H1B 1.00 . ?
C1A C9A 1.429(2) . ?
C1A C2A 1.432(2) . ?
C1A C5A 1.438(2) . ?
C2A C6A 1.432(2) . ?
C2A C3A 1.4353(15) . ?
C3A C4A 1.4297(15) . ?
C4A C5A 1.4252(15) . ?
C6A C7A 1.371(2) . ?
C7A C8A 1.428(2) . ?
C8A C9A 1.376(2) . ?
C1B C9B 1.4268(15) . ?
C1B C5B 1.430(2) . ?
C1B C2B 1.4394(15) . ?
C2B C6B 1.4320(15) . ?
C2B C3B 1.4368(15) . ?
C3B C4B 1.4333(15) . ?
C4B C5B 1.4313(15) . ?
C6B C7B 1.372(2) . ?
C7B C8B 1.430(2) . ?
C8B C9B 1.373(2) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10A Si1A C4A C3A 179.26(10) . . . . ?
C11A Si1A C4A C3A 59.30(12) . . . . ?
C10B Si1B C4B C3B 163.23(11) . . . . ?
C11B Si1B C4B C3B 41.68(12) . . . . ?
