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)
Lee, Hyosun; Bridgewater, Brian M.; Parkin, Gerard; Journal of the Chemical Society, Dalton Transactions  (2000) 4490–; doi:10.1039/b005117i

data_7010024
_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&#x2005;=&#x2005;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            'C28 H37 N Zr'
_chemical_formula_weight         478.81
_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                89.3260(10)
_cell_angle_beta                 79.892(2)
_cell_angle_gamma                70.0910(10)
_cell_formula_units_Z            2
_cell_length_a                   8.7032(7)
_cell_length_b                   9.6822(8)
_cell_length_c                   15.8118(12)
_cell_measurement_temperature    223(2)
_cell_volume                     1231.66(17)
_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 0.822
_diffrn_measured_fraction_theta_max 0.822
_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  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0638
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6631
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    0.460
_exptl_absorpt_correction_T_max  0.9774
_exptl_absorpt_correction_T_min  0.9554
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.0000(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         5018
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          1.007
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1075
_reflns_number_gt                3903
_reflns_number_total             5018
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b005117i.txt
_cod_data_source_block           hbs10
_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               7010024