Zirconium Sandwich Complexes with η9 Indenyl Ligands: Well-Defined Precursors for Zirconocene-Mediated Coupling Reactions
Christopher A. Bradley; Ivan Keresztes; Emil Lobkovsky; Victor G. Young; Paul J. Chirik; Journal of the American Chemical Society 126 (2004) 16937–16950; doi:10.1021/ja045072v

data_4113340
_publ_section_title
;
 Zirconium Sandwich Complexes with \h9 Indenyl Ligands: Well-Defined
 Precursors for Zirconocene-Mediated Coupling Reactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16937
_journal_page_last               16950
_journal_paper_doi               10.1021/ja045072v
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C30 H38 Zr'
_chemical_formula_weight         489.82
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.1150(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8131(6)
_cell_length_b                   13.2683(7)
_cell_length_c                   17.2953(9)
_cell_measurement_temperature    173(2)
_cell_volume                     2475.0(2)
_computing_cell_refinement       'Bruker SAINT'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.910
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'Bruker 1K CCD area detector'
_diffrn_measurement_method       '0.3 deg. 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  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0731
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19802
_diffrn_reflns_theta_full        31.85
_diffrn_reflns_theta_max         31.85
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    0.459
_exptl_absorpt_correction_T_max  0.9556
_exptl_absorpt_correction_T_min  0.8378
_exptl_absorpt_correction_type   'semiempirical by SADABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    isotropic
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         7725
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.139
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+0.4466P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0860
_reflns_number_gt                5305
_reflns_number_total             7725
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja045072vsi20040816_023353.cif
_cod_data_source_block           cb47
_cod_database_code               4113340