#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:13:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179804 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/00/7010023.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_7010023
loop_
_publ_author_name
'Lee, Hyosun'
'Bridgewater, Brian M.'
'Parkin, Gerard'
_publ_section_title
;
 Influence of a [Me2Si] ansa bridge on the barrier to rotation about
 the Zr--phenyl bond and on the generation and reactivity of benzyne
 intermediates: comparison of the structures and reactivity of
 [Me2Si(C5Me4)2]Zr(Ph)X and Cp*2Zr(Ph)X (X = H, Cl, Ph)
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4490
_journal_paper_doi               10.1039/b005117i
_journal_year                    2000
_chemical_formula_sum            'C26 H35 Cl Si Zr'
_chemical_formula_weight         502.30
_chemical_name_systematic
; 
 ? 
;
_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                 91.1940(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6955(4)
_cell_length_b                   12.4482(6)
_cell_length_c                   20.4091(9)
_cell_measurement_temperature    203(2)
_cell_volume                     2462.67(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17993
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.614
_exptl_absorpt_correction_T_max  0.9700
_exptl_absorpt_correction_T_min  0.8871
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.00000(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         5689
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.119
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0419P)²+0.7821P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0829
_reflns_number_gt                4560
_reflns_number_total             5689
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b005117i.txt
_cod_data_source_block           azrs20
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7010023
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_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 0.20576(2) 0.778462(16) 0.143643(9) 0.02635(7) Uani 1 1 d . . .
Si Si -0.11009(6) 0.68345(5) 0.15849(3) 0.03120(14) Uani 1 1 d . . .
Cl Cl 0.30785(8) 0.92491(5) 0.20830(3) 0.05165(17) Uani 1 1 d . . .
C1 C -0.2007(3) 0.5711(2) 0.11507(13) 0.0447(6) Uani 1 1 d . . .
H1A H -0.2222 0.5150 0.1462 0.067 Uiso 1 1 calc R . .
H1B H -0.1416 0.5422 0.0816 0.067 Uiso 1 1 calc R . .
H1C H -0.2854 0.5976 0.0948 0.067 Uiso 1 1 calc R . .
C2 C -0.2410(3) 0.7312(2) 0.21793(14) 0.0491(6) Uani 1 1 d . . .
H2A H -0.3228 0.7556 0.1941 0.074 Uiso 1 1 calc R . .
H2B H -0.2028 0.7900 0.2436 0.074 Uiso 1 1 calc R . .
H2C H -0.2653 0.6726 0.2469 0.074 Uiso 1 1 calc R . .
C11 C -0.0371(2) 0.79136(17) 0.10386(10) 0.0296(4) Uani 1 1 d . . .
C12 C 0.0416(2) 0.77154(17) 0.04577(10) 0.0305(4) Uani 1 1 d . . .
C13 C 0.1237(2) 0.86277(18) 0.03279(10) 0.0321(5) Uani 1 1 d . . .
C14 C 0.0990(2) 0.94048(17) 0.08192(11) 0.0334(5) Uani 1 1 d . . .
C15 C 0.0006(2) 0.89759(17) 0.12523(11) 0.0321(5) Uani 1 1 d . . .
C21 C 0.0603(2) 0.64404(17) 0.19792(10) 0.0290(4) Uani 1 1 d . . .
C22 C 0.1646(2) 0.58137(17) 0.16621(10) 0.0298(4) Uani 1 1 d . . .
C23 C 0.2936(2) 0.59966(18) 0.19782(11) 0.0335(5) Uani 1 1 d . . .
C24 C 0.2734(2) 0.6729(2) 0.24960(11) 0.0357(5) Uani 1 1 d . . .
C25 C 0.1311(2) 0.70098(18) 0.24988(10) 0.0321(5) Uani 1 1 d . . .
C32 C 0.0238(3) 0.6803(2) -0.00166(12) 0.0406(5) Uani 1 1 d . . .
H32A H -0.0309 0.7041 -0.0393 0.061 Uiso 1 1 calc R . .
H32B H -0.0227 0.6213 0.0196 0.061 Uiso 1 1 calc R . .
H32C H 0.1136 0.6567 -0.0160 0.061 Uiso 1 1 calc R . .
C33 C 0.2092(3) 0.8819(2) -0.02653(11) 0.0426(6) Uani 1 1 d . . .
H33A H 0.1585 0.9273 -0.0572 0.064 Uiso 1 1 calc R . .
H33B H 0.2295 0.8137 -0.0472 0.064 Uiso 1 1 calc R . .
H33C H 0.2947 0.9170 -0.0135 0.064 Uiso 1 1 calc R . .
C34 C 0.1588(3) 1.05148(19) 0.08332(13) 0.0467(6) Uani 1 1 d . . .
H34A H 0.2562 1.0480 0.0737 0.070 Uiso 1 1 calc R . .
H34B H 0.1473 1.0826 0.1264 0.070 Uiso 1 1 calc R . .
H34C H 0.1116 1.0957 0.0508 0.070 Uiso 1 1 calc R . .
C35 C -0.0598(3) 0.9610(2) 0.18047(12) 0.0453(6) Uani 1 1 d . . .
H35A H -0.0787 0.9133 0.2168 0.068 Uiso 1 1 calc R . .
H35B H -0.1450 0.9947 0.1655 0.068 Uiso 1 1 calc R . .
H35C H 0.0052 1.0159 0.1947 0.068 Uiso 1 1 calc R . .
C42 C 0.1429(3) 0.49350(19) 0.11623(12) 0.0398(5) Uani 1 1 d . . .
H42A H 0.2089 0.5016 0.0815 0.060 Uiso 1 1 calc R . .
H42B H 0.0500 0.4982 0.0979 0.060 Uiso 1 1 calc R . .
H42C H 0.1557 0.4241 0.1372 0.060 Uiso 1 1 calc R . .
C43 C 0.4243(3) 0.5395(2) 0.18523(14) 0.0482(6) Uani 1 1 d . . .
H43A H 0.5027 0.5819 0.2003 0.072 Uiso 1 1 calc R . .
H43B H 0.4316 0.5260 0.1386 0.072 Uiso 1 1 calc R . .
H43C H 0.4233 0.4716 0.2086 0.072 Uiso 1 1 calc R . .
C44 C 0.3809(3) 0.7065(3) 0.29992(13) 0.0519(7) Uani 1 1 d . . .
H44A H 0.3850 0.6540 0.3350 0.078 Uiso 1 1 calc R . .
H44B H 0.3566 0.7761 0.3177 0.078 Uiso 1 1 calc R . .
H44C H 0.4701 0.7111 0.2795 0.078 Uiso 1 1 calc R . .
C45 C 0.0695(3) 0.7710(2) 0.30177(12) 0.0433(6) Uani 1 1 d . . .
H45A H 0.0570 0.7292 0.3413 0.065 Uiso 1 1 calc R . .
H45B H -0.0191 0.7981 0.2862 0.065 Uiso 1 1 calc R . .
H45C H 0.1308 0.8308 0.3112 0.065 Uiso 1 1 calc R . .
C51 C 0.3835(2) 0.7399(2) 0.07545(12) 0.0390(5) Uani 1 1 d . . .
C52 C 0.3927(3) 0.6602(2) 0.02795(14) 0.0500(7) Uani 1 1 d . . .
H52A H 0.3234 0.6075 0.0256 0.060 Uiso 1 1 calc R . .
C53 C 0.4999(3) 0.6549(3) -0.01620(15) 0.0618(8) Uani 1 1 d . . .
H53A H 0.5013 0.5996 -0.0476 0.074 Uiso 1 1 calc R . .
C54 C 0.6034(3) 0.7297(3) -0.01424(18) 0.0688(10) Uani 1 1 d . . .
H54A H 0.6745 0.7275 -0.0448 0.083 Uiso 1 1 calc R . .
C55 C 0.6015(3) 0.8082(3) 0.03341(17) 0.0657(9) Uani 1 1 d . . .
H55A H 0.6738 0.8584 0.0364 0.079 Uiso 1 1 calc R . .
C56 C 0.4938(3) 0.8136(2) 0.07685(14) 0.0505(7) Uani 1 1 d . . .
H56A H 0.4943 0.8685 0.1085 0.061 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 0.0000 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
C51 Zr Cl 100.55(7) . . ?
C51 Zr C21 125.14(8) . . ?
Cl Zr C21 119.46(5) . . ?
C51 Zr C11 122.43(8) . . ?
Cl Zr C11 119.93(5) . . ?
C21 Zr C11 69.09(7) . . ?
C51 Zr C25 133.10(8) . . ?
Cl Zr C25 86.60(5) . . ?
C21 Zr C25 33.70(7) . . ?
C11 Zr C25 91.09(7) . . ?
C51 Zr C15 129.73(8) . . ?
Cl Zr C15 87.18(5) . . ?
C21 Zr C15 90.54(7) . . ?
C11 Zr C15 33.53(7) . . ?
C25 Zr C15 96.64(7) . . ?
C51 Zr C12 88.96(8) . . ?
Cl Zr C12 133.78(5) . . ?
C21 Zr C12 88.58(7) . . ?
C11 Zr C12 33.50(7) . . ?
C25 Zr C12 118.96(7) . . ?
C15 Zr C12 54.32(7) . . ?
C51 Zr C22 91.76(8) . . ?
Cl Zr C22 133.46(5) . . ?
C21 Zr C22 33.50(7) . . ?
C11 Zr C22 88.28(7) . . ?
C25 Zr C22 54.33(7) . . ?
C15 Zr C22 118.29(7) . . ?
C12 Zr C22 90.66(7) . . ?
C51 Zr C14 99.59(8) . . ?
Cl Zr C14 80.49(6) . . ?
C21 Zr C14 121.45(7) . . ?
C11 Zr C14 54.66(7) . . ?
C25 Zr C14 127.25(7) . . ?
C15 Zr C14 32.33(7) . . ?
C12 Zr C14 53.29(7) . . ?
C22 Zr C14 141.53(7) . . ?
C51 Zr C24 102.67(8) . . ?
Cl Zr C24 80.56(6) . . ?
C21 Zr C24 54.61(7) . . ?
C11 Zr C24 121.73(7) . . ?
C25 Zr C24 32.35(7) . . ?
C15 Zr C24 127.57(7) . . ?
C12 Zr C24 141.49(7) . . ?
C22 Zr C24 52.92(7) . . ?
C14 Zr C24 153.00(7) . . ?
C51 Zr C13 77.08(8) . . ?
Cl Zr C13 106.33(5) . . ?
C21 Zr C13 119.78(7) . . ?
C11 Zr C13 54.44(7) . . ?
C25 Zr C13 145.33(7) . . ?
C15 Zr C13 53.36(7) . . ?
C12 Zr C13 31.96(7) . . ?
C22 Zr C13 120.17(7) . . ?
C14 Zr C13 31.71(7) . . ?
C24 Zr C13 173.07(7) . . ?
C51 Zr C23 80.56(7) . . ?
Cl Zr C23 106.32(6) . . ?
C21 Zr C23 54.39(7) . . ?
C11 Zr C23 119.43(7) . . ?
C25 Zr C23 53.28(7) . . ?
C15 Zr C23 144.79(7) . . ?
C12 Zr C23 119.87(7) . . ?
C22 Zr C23 31.82(7) . . ?
C14 Zr C23 173.08(7) . . ?
C24 Zr C23 31.37(7) . . ?
C13 Zr C23 143.14(7) . . ?
C1 Si C2 103.11(12) . . ?
C1 Si C21 114.01(11) . . ?
C2 Si C21 113.93(11) . . ?
C1 Si C11 115.50(11) . . ?
C2 Si C11 115.09(11) . . ?
C21 Si C11 95.79(9) . . ?
C15 C11 C12 105.73(18) . . ?
C15 C11 Si 124.76(16) . . ?
C12 C11 Si 124.94(16) . . ?
C15 C11 Zr 74.14(12) . . ?
C12 C11 Zr 75.14(12) . . ?
Si C11 Zr 97.21(9) . . ?
C13 C12 C11 108.99(18) . . ?
C13 C12 C32 123.0(2) . . ?
C11 C12 C32 127.1(2) . . ?
C13 C12 Zr 76.90(13) . . ?
C11 C12 Zr 71.36(12) . . ?
C32 C12 Zr 126.70(16) . . ?
C12 C13 C14 108.13(18) . . ?
C12 C13 C33 126.9(2) . . ?
C14 C13 C33 124.6(2) . . ?
C12 C13 Zr 71.13(12) . . ?
C14 C13 Zr 73.35(12) . . ?
C33 C13 Zr 126.97(16) . . ?
C13 C14 C15 108.05(19) . . ?
C13 C14 C34 124.9(2) . . ?
C15 C14 C34 126.9(2) . . ?
C13 C14 Zr 74.93(12) . . ?
C15 C14 Zr 70.73(12) . . ?
C34 C14 Zr 124.03(17) . . ?
C14 C15 C11 109.10(18) . . ?
C14 C15 C35 123.2(2) . . ?
C11 C15 C35 127.5(2) . . ?
C14 C15 Zr 76.94(13) . . ?
C11 C15 Zr 72.34(12) . . ?
C35 C15 Zr 121.26(16) . . ?
C25 C21 C22 105.62(19) . . ?
C25 C21 Si 125.91(16) . . ?
C22 C21 Si 124.42(16) . . ?
C25 C21 Zr 74.22(11) . . ?
C22 C21 Zr 75.67(11) . . ?
Si C21 Zr 97.80(8) . . ?
C23 C22 C21 109.27(19) . . ?
C23 C22 C42 122.4(2) . . ?
C21 C22 C42 127.4(2) . . ?
C23 C22 Zr 77.60(12) . . ?
C21 C22 Zr 70.83(11) . . ?
C42 C22 Zr 126.94(15) . . ?
C24 C23 C22 108.09(19) . . ?
C24 C23 C43 125.5(2) . . ?
C22 C23 C43 125.8(2) . . ?
C24 C23 Zr 73.66(13) . . ?
C22 C23 Zr 70.58(12) . . ?
C43 C23 Zr 128.37(15) . . ?
C23 C24 C25 108.1(2) . . ?
C23 C24 C44 125.8(2) . . ?
C25 C24 C44 125.8(2) . . ?
C23 C24 Zr 74.97(12) . . ?
C25 C24 Zr 69.62(12) . . ?
C44 C24 Zr 125.79(16) . . ?
C24 C25 C21 108.90(19) . . ?
C24 C25 C45 123.0(2) . . ?
C21 C25 C45 127.9(2) . . ?
C24 C25 Zr 78.03(12) . . ?
C21 C25 Zr 72.08(11) . . ?
C45 C25 Zr 120.96(15) . . ?
C52 C51 C56 114.7(2) . . ?
C52 C51 Zr 129.35(18) . . ?
C56 C51 Zr 115.58(19) . . ?
C51 C52 C53 123.1(3) . . ?
C54 C53 C52 120.4(3) . . ?
C53 C54 C55 118.8(3) . . ?
C54 C55 C56 120.4(3) . . ?
C55 C56 C51 122.5(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 C51 2.288(2) . ?
Zr Cl 2.4475(6) . ?
Zr C21 2.4661(19) . ?
Zr C11 2.480(2) . ?
Zr C25 2.494(2) . ?
Zr C15 2.503(2) . ?
Zr C12 2.529(2) . ?
Zr C22 2.530(2) . ?
Zr C14 2.583(2) . ?
Zr C24 2.603(2) . ?
Zr C13 2.603(2) . ?
Zr C23 2.620(2) . ?
Si C1 1.866(2) . ?
Si C2 1.871(2) . ?
Si C21 1.887(2) . ?
Si C11 1.893(2) . ?
C11 C15 1.437(3) . ?
C11 C12 1.444(3) . ?
C12 C13 1.415(3) . ?
C12 C32 1.499(3) . ?
C13 C14 1.417(3) . ?
C13 C33 1.500(3) . ?
C14 C15 1.418(3) . ?
C14 C34 1.499(3) . ?
C15 C35 1.505(3) . ?
C21 C25 1.438(3) . ?
C21 C22 1.441(3) . ?
C22 C23 1.414(3) . ?
C22 C42 1.507(3) . ?
C23 C24 1.412(3) . ?
C23 C43 1.499(3) . ?
C24 C25 1.424(3) . ?
C24 C44 1.507(3) . ?
C25 C45 1.505(3) . ?
C51 C52 1.391(4) . ?
C51 C56 1.409(4) . ?
C52 C53 1.391(3) . ?
C53 C54 1.369(5) . ?
C54 C55 1.379(5) . ?
C55 C56 1.386(4) . ?
