#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:13:34 +0100 (vie 25 de mar de 2016) $
#$Revision: 179804 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/00/7010028.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_7010028
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            'C30 H40 N2 Si Zr'
_chemical_formula_weight         547.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                83.5780(10)
_cell_angle_beta                 78.9870(10)
_cell_angle_gamma                74.4950(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4411(5)
_cell_length_b                   10.2964(6)
_cell_length_c                   14.6641(8)
_cell_measurement_temperature    223(2)
_cell_volume                     1345.53(13)
_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      223(2)
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.903
_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  0.0163
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10239
_diffrn_reflns_theta_full        28.21
_diffrn_reflns_theta_max         28.21
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    0.474
_exptl_absorpt_correction_T_max  0.9541
_exptl_absorpt_correction_T_min  0.9112
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.985
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0000(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         5989
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          4.365
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0561P)²+1.4446P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1197
_reflns_number_gt                5095
_reflns_number_total             5989
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b005117i.txt
_cod_data_source_block           zrms10
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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      P-1
_cod_database_code               7010028
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 0.74373(3) 0.70364(3) 0.753655(19) 0.03441(11) Uani 1 1 d . . .
N1 N 0.7887(4) 0.8667(3) 0.8216(2) 0.0597(8) Uani 1 1 d . . .
N2 N 0.9570(4) 0.6843(4) 0.8224(2) 0.0605(8) Uani 1 1 d . . .
H2A H 1.0361 0.6184 0.8259 0.073 Uiso 1 1 calc R . .
C11 C 0.8303(3) 0.5810(3) 0.6067(2) 0.0353(6) Uani 1 1 d . . .
C12 C 0.7262(3) 0.7049(3) 0.5815(2) 0.0389(6) Uani 1 1 d . . .
C13 C 0.7871(4) 0.8155(3) 0.5853(2) 0.0422(7) Uani 1 1 d . . .
C14 C 0.9285(4) 0.7641(3) 0.6123(2) 0.0424(7) Uani 1 1 d . . .
C15 C 0.9562(3) 0.6211(3) 0.6242(2) 0.0387(6) Uani 1 1 d . . .
C21 C 0.6938(3) 0.4732(3) 0.7774(2) 0.0352(6) Uani 1 1 d . . .
C22 C 0.5498(3) 0.5656(3) 0.8011(2) 0.0414(7) Uani 1 1 d . . .
C23 C 0.5463(4) 0.6267(3) 0.8834(2) 0.0447(7) Uani 1 1 d . . .
C24 C 0.6847(4) 0.5754(3) 0.9128(2) 0.0437(7) Uani 1 1 d . . .
C25 C 0.7749(3) 0.4802(3) 0.8492(2) 0.0383(6) Uani 1 1 d . . .
C32 C 0.5904(4) 0.7181(4) 0.5383(3) 0.0534(8) Uani 1 1 d . . .
H32A H 0.5146 0.7981 0.5591 0.080 Uiso 1 1 calc R . .
H32B H 0.5520 0.6389 0.5569 0.080 Uiso 1 1 calc R . .
H32C H 0.6170 0.7259 0.4710 0.080 Uiso 1 1 calc R . .
C33 C 0.7216(5) 0.9594(4) 0.5554(3) 0.0607(10) Uani 1 1 d . . .
H33A H 0.7609 1.0183 0.5853 0.091 Uiso 1 1 calc R . .
H33B H 0.6140 0.9804 0.5731 0.091 Uiso 1 1 calc R . .
H33C H 0.7475 0.9727 0.4884 0.091 Uiso 1 1 calc R . .
C34 C 1.0353(5) 0.8460(4) 0.6186(3) 0.0606(10) Uani 1 1 d . . .
H34A H 1.1081 0.7953 0.6564 0.091 Uiso 1 1 calc R . .
H34B H 0.9810 0.9298 0.6469 0.091 Uiso 1 1 calc R . .
H34C H 1.0860 0.8660 0.5567 0.091 Uiso 1 1 calc R . .
C35 C 1.1038(4) 0.5291(4) 0.6414(3) 0.0509(8) Uani 1 1 d . . .
H35A H 1.1683 0.5828 0.6524 0.076 Uiso 1 1 calc R . .
H35B H 1.1504 0.4773 0.5874 0.076 Uiso 1 1 calc R . .
H35C H 1.0875 0.4680 0.6955 0.076 Uiso 1 1 calc R . .
C42 C 0.4144(4) 0.5747(4) 0.7581(3) 0.0560(9) Uani 1 1 d . . .
H42A H 0.3887 0.4885 0.7683 0.084 Uiso 1 1 calc R . .
H42B H 0.4360 0.5973 0.6917 0.084 Uiso 1 1 calc R . .
H42C H 0.3315 0.6441 0.7865 0.084 Uiso 1 1 calc R . .
C43 C 0.4148(5) 0.7203(4) 0.9380(3) 0.0656(11) Uani 1 1 d . . .
H43A H 0.3354 0.7507 0.9013 0.098 Uiso 1 1 calc R . .
H43B H 0.4445 0.7976 0.9528 0.098 Uiso 1 1 calc R . .
H43C H 0.3797 0.6728 0.9953 0.098 Uiso 1 1 calc R . .
C44 C 0.7236(5) 0.6066(4) 1.0017(2) 0.0623(10) Uani 1 1 d . . .
H44A H 0.6682 0.5659 1.0546 0.093 Uiso 1 1 calc R . .
H44B H 0.6980 0.7037 1.0062 0.093 Uiso 1 1 calc R . .
H44C H 0.8297 0.5704 1.0015 0.093 Uiso 1 1 calc R . .
C45 C 0.9248(4) 0.3903(4) 0.8634(3) 0.0526(8) Uani 1 1 d . . .
H45A H 1.0012 0.4109 0.8138 0.079 Uiso 1 1 calc R . .
H45B H 0.9235 0.2965 0.8626 0.079 Uiso 1 1 calc R . .
H45C H 0.9460 0.4056 0.9229 0.079 Uiso 1 1 calc R . .
C51 C 0.9424(5) 0.2687(4) 0.6479(3) 0.0601(10) Uani 1 1 d . . .
H51A H 0.9104 0.1899 0.6775 0.090 Uiso 1 1 calc R . .
H51B H 1.0176 0.2843 0.6791 0.090 Uiso 1 1 calc R . .
H51C H 0.9839 0.2538 0.5830 0.090 Uiso 1 1 calc R . .
C52 C 0.6462(5) 0.3690(4) 0.5960(3) 0.0582(9) Uani 1 1 d . . .
H52A H 0.5590 0.4439 0.5929 0.087 Uiso 1 1 calc R . .
H52B H 0.6160 0.2922 0.6306 0.087 Uiso 1 1 calc R . .
H52C H 0.6943 0.3448 0.5335 0.087 Uiso 1 1 calc R . .
C61 C 0.5440(4) 0.8974(3) 0.7590(2) 0.0467(7) Uani 1 1 d . . .
C62 C 0.4089(4) 0.9154(4) 0.7269(3) 0.0606(10) Uani 1 1 d . . .
H62A H 0.3921 0.8420 0.7016 0.073 Uiso 1 1 calc R . .
C63 C 0.2989(5) 1.0354(5) 0.7305(4) 0.0830(15) Uani 1 1 d . . .
H63A H 0.2100 1.0423 0.7083 0.100 Uiso 1 1 calc R . .
C64 C 0.3213(6) 1.1446(6) 0.7668(5) 0.104(2) Uani 1 1 d . . .
H64A H 0.2467 1.2262 0.7704 0.124 Uiso 1 1 calc R . .
C65 C 0.4526(7) 1.1344(5) 0.7979(4) 0.0873(16) Uani 1 1 d . . .
H65A H 0.4684 1.2097 0.8214 0.105 Uiso 1 1 calc R . .
C66 C 0.5632(4) 1.0122(4) 0.7946(3) 0.0565(9) Uani 1 1 d . . .
C71 C 0.7473(8) 1.1029(6) 0.8523(5) 0.106(2) Uani 1 1 d . . .
H71A H 0.8426 1.0877 0.8681 0.128 Uiso 1 1 calc R . .
H71B H 0.6827 1.1900 0.8540 0.128 Uiso 1 1 calc R . .
C72 C 0.7039(6) 1.0007(4) 0.8272(3) 0.0685(11) Uani 1 1 d . . .
C81 C 0.9883(6) 0.8620(6) 0.9131(4) 0.0909(16) Uani 1 1 d . . .
H81A H 1.0591 0.7912 0.9422 0.136 Uiso 1 1 calc R . .
H81B H 0.9122 0.9094 0.9608 0.136 Uiso 1 1 calc R . .
H81C H 1.0398 0.9250 0.8760 0.136 Uiso 1 1 calc R . .
C82 C 0.9179(5) 0.8018(4) 0.8524(3) 0.0573(9) Uani 1 1 d . . .
Si Si 0.77905(10) 0.41947(8) 0.65563(6) 0.03820(19) Uani 1 1 d . . .
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'
N N 0.0061 0.0033 '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'
Si Si 0.0817 0.0704 '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
N1 Zr C61 68.66(13) . . ?
N1 Zr N2 54.68(12) . . ?
C61 Zr N2 123.22(13) . . ?
N1 Zr C11 140.06(11) . . ?
C61 Zr C11 119.09(11) . . ?
N2 Zr C11 107.24(11) . . ?
N1 Zr C21 145.26(11) . . ?
C61 Zr C21 119.96(11) . . ?
N2 Zr C21 105.67(11) . . ?
C11 Zr C21 68.89(10) . . ?
N1 Zr C15 109.75(11) . . ?
C61 Zr C15 130.60(11) . . ?
N2 Zr C15 77.09(11) . . ?
C11 Zr C15 33.11(9) . . ?
C21 Zr C15 89.82(10) . . ?
N1 Zr C25 114.15(11) . . ?
C61 Zr C25 131.31(11) . . ?
N2 Zr C25 75.43(11) . . ?
C11 Zr C25 90.18(10) . . ?
C21 Zr C25 32.97(9) . . ?
C15 Zr C25 95.65(10) . . ?
N1 Zr C22 131.76(12) . . ?
C61 Zr C22 87.36(11) . . ?
N2 Zr C22 126.77(11) . . ?
C11 Zr C22 88.11(10) . . ?
C21 Zr C22 32.99(10) . . ?
C15 Zr C22 117.42(11) . . ?
C25 Zr C22 53.33(10) . . ?
N1 Zr C12 126.15(11) . . ?
C61 Zr C12 86.29(11) . . ?
N2 Zr C12 128.87(11) . . ?
C11 Zr C12 33.17(9) . . ?
C21 Zr C12 88.59(10) . . ?
C15 Zr C12 53.65(9) . . ?
C25 Zr C12 118.02(10) . . ?
C22 Zr C12 91.33(10) . . ?
N1 Zr C14 85.81(11) . . ?
C61 Zr C14 102.21(11) . . ?
N2 Zr C14 78.71(11) . . ?
C11 Zr C14 54.46(10) . . ?
C21 Zr C14 120.91(10) . . ?
C15 Zr C14 32.37(10) . . ?
C25 Zr C14 126.32(10) . . ?
C22 Zr C14 141.46(10) . . ?
C12 Zr C14 52.92(10) . . ?
N1 Zr C24 91.55(11) . . ?
C61 Zr C24 103.04(11) . . ?
N2 Zr C24 76.82(11) . . ?
C11 Zr C24 120.88(10) . . ?
C21 Zr C24 54.18(10) . . ?
C15 Zr C24 126.18(10) . . ?
C25 Zr C24 32.11(10) . . ?
C22 Zr C24 52.67(10) . . ?
C12 Zr C24 141.49(10) . . ?
C14 Zr C24 151.67(11) . . ?
N1 Zr C13 94.90(12) . . ?
C61 Zr C13 77.53(11) . . ?
N2 Zr C13 108.63(11) . . ?
C11 Zr C13 54.20(10) . . ?
C21 Zr C13 119.58(10) . . ?
C15 Zr C13 53.11(10) . . ?
C25 Zr C13 144.16(10) . . ?
C22 Zr C13 120.86(10) . . ?
C12 Zr C13 31.79(10) . . ?
C14 Zr C13 31.59(10) . . ?
C24 Zr C13 173.24(10) . . ?
C82 N1 C72 131.4(4) . . ?
C82 N1 Zr 101.4(2) . . ?
C72 N1 Zr 127.2(3) . . ?
C82 N2 Zr 96.8(3) . . ?
C15 C11 C12 105.5(3) . . ?
C15 C11 Si 124.7(2) . . ?
C12 C11 Si 125.1(2) . . ?
C15 C11 Zr 73.88(16) . . ?
C12 C11 Zr 75.39(16) . . ?
Si C11 Zr 96.93(12) . . ?
C13 C12 C11 109.1(3) . . ?
C13 C12 C32 122.7(3) . . ?
C11 C12 C32 127.0(3) . . ?
C13 C12 Zr 76.11(18) . . ?
C11 C12 Zr 71.45(16) . . ?
C32 C12 Zr 128.6(2) . . ?
C14 C13 C12 108.0(3) . . ?
C14 C13 C33 125.7(3) . . ?
C12 C13 C33 125.9(3) . . ?
C14 C13 Zr 72.86(17) . . ?
C12 C13 Zr 72.10(17) . . ?
C33 C13 Zr 126.1(2) . . ?
C13 C14 C15 108.1(3) . . ?
C13 C14 C34 125.4(3) . . ?
C15 C14 C34 126.3(3) . . ?
C13 C14 Zr 75.55(17) . . ?
C15 C14 Zr 71.58(17) . . ?
C34 C14 Zr 122.8(2) . . ?
C14 C15 C11 109.3(3) . . ?
C14 C15 C35 123.6(3) . . ?
C11 C15 C35 126.7(3) . . ?
C14 C15 Zr 76.05(17) . . ?
C11 C15 Zr 73.01(16) . . ?
C35 C15 Zr 122.9(2) . . ?
C25 C21 C22 105.3(3) . . ?
C25 C21 Si 125.7(2) . . ?
C22 C21 Si 124.2(2) . . ?
C25 C21 Zr 74.22(16) . . ?
C22 C21 Zr 75.14(16) . . ?
Si C21 Zr 96.49(12) . . ?
C23 C22 C21 109.0(3) . . ?
C23 C22 C42 124.3(3) . . ?
C21 C22 C42 125.6(3) . . ?
C23 C22 Zr 76.25(18) . . ?
C21 C22 Zr 71.87(16) . . ?
C42 C22 Zr 127.9(2) . . ?
C24 C23 C22 108.4(3) . . ?
C24 C23 C43 123.9(3) . . ?
C22 C23 C43 127.4(3) . . ?
C24 C23 Zr 73.50(18) . . ?
C22 C23 Zr 72.05(17) . . ?
C43 C23 Zr 125.0(2) . . ?
C23 C24 C25 107.9(3) . . ?
C23 C24 C44 125.4(3) . . ?
C25 C24 C44 126.5(3) . . ?
C23 C24 Zr 75.22(18) . . ?
C25 C24 Zr 71.75(17) . . ?
C44 C24 Zr 123.4(2) . . ?
C24 C25 C21 109.3(3) . . ?
C24 C25 C45 123.9(3) . . ?
C21 C25 C45 126.4(3) . . ?
C24 C25 Zr 76.14(17) . . ?
C21 C25 Zr 72.81(16) . . ?
C45 C25 Zr 123.1(2) . . ?
C62 C61 C66 115.4(3) . . ?
C62 C61 Zr 127.6(3) . . ?
C66 C61 Zr 116.9(3) . . ?
C63 C62 C61 123.5(4) . . ?
C64 C63 C62 119.3(5) . . ?
C65 C64 C63 120.0(4) . . ?
C64 C65 C66 120.3(5) . . ?
C65 C66 C61 121.4(4) . . ?
C65 C66 C72 120.7(4) . . ?
C61 C66 C72 117.9(3) . . ?
C71 C72 N1 125.8(5) . . ?
C71 C72 C66 125.5(5) . . ?
N1 C72 C66 108.5(3) . . ?
N2 C82 N1 106.9(3) . . ?
N2 C82 C81 129.5(4) . . ?
N1 C82 C81 123.5(4) . . ?
N2 C82 Zr 56.7(2) . . ?
N1 C82 Zr 50.41(19) . . ?
C81 C82 Zr 171.5(3) . . ?
C52 Si C51 103.18(19) . . ?
C52 Si C11 115.26(16) . . ?
C51 Si C11 113.21(17) . . ?
C52 Si C21 112.76(16) . . ?
C51 Si C21 115.38(16) . . ?
C11 Si C21 97.62(13) . . ?
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 N1 2.216(3) . ?
Zr C61 2.348(3) . ?
Zr N2 2.372(3) . ?
Zr C11 2.508(3) . ?
Zr C21 2.514(3) . ?
Zr C15 2.519(3) . ?
Zr C25 2.533(3) . ?
Zr C22 2.557(3) . ?
Zr C12 2.560(3) . ?
Zr C14 2.577(3) . ?
Zr C24 2.589(3) . ?
Zr C13 2.611(3) . ?
N1 C82 1.359(5) . ?
N1 C72 1.400(5) . ?
N2 C82 1.269(5) . ?
C11 C15 1.432(4) . ?
C11 C12 1.447(4) . ?
C11 Si 1.883(3) . ?
C12 C13 1.417(5) . ?
C12 C32 1.504(4) . ?
C13 C14 1.412(5) . ?
C13 C33 1.496(4) . ?
C14 C15 1.422(4) . ?
C14 C34 1.498(5) . ?
C15 C35 1.509(4) . ?
C21 C25 1.432(4) . ?
C21 C22 1.441(4) . ?
C21 Si 1.891(3) . ?
C22 C23 1.413(5) . ?
C22 C42 1.507(4) . ?
C23 C24 1.402(5) . ?
C23 C43 1.505(5) . ?
C24 C25 1.418(4) . ?
C24 C44 1.510(5) . ?
C25 C45 1.508(4) . ?
C51 Si 1.869(4) . ?
C52 Si 1.865(3) . ?
C61 C62 1.402(5) . ?
C61 C66 1.411(5) . ?
C62 C63 1.384(5) . ?
C63 C64 1.377(8) . ?
C64 C65 1.376(8) . ?
C65 C66 1.403(6) . ?
C66 C72 1.467(6) . ?
C71 C72 1.337(6) . ?
C81 C82 1.480(5) . ?
