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_4113341
_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            'C84 H132 Si8 Zr2'
_chemical_formula_weight         1548.05
_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                73.100(2)
_cell_angle_beta                 76.224(2)
_cell_angle_gamma                80.831(2)
_cell_formula_units_Z            2
_cell_length_a                   15.7325(13)
_cell_length_b                   17.0445(15)
_cell_length_c                   17.9558(15)
_cell_measurement_temperature    173(2)
_cell_volume                     4453.3(7)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker 1K CCD'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0920
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19407
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    0.380
_exptl_absorpt_correction_T_max  0.9278
_exptl_absorpt_correction_T_min  0.8628
_exptl_absorpt_correction_type   'semiempirical by SADABS'
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_description       block
_exptl_crystal_F_000             1654
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.183
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     986
_refine_ls_number_reflns         19407
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.185
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+3.2200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1379
_reflns_number_gt                13008
_reflns_number_total             19407
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja045072vsi20040819_010126.cif
_cod_data_source_block           cb44
_cod_database_code               4113341