Carbon-Oxygen Bond Cleavage with η9,η5-Bis(indenyl)zirconium Sandwich Complexes
Christopher A. Bradley; Luis F. Veiros; Doris Pun; Emil Lobkovsky; Ivan Keresztes; Paul J. Chirik; Journal of the American Chemical Society 128 (2006) 16600–16612; doi:10.1021/ja065456g

data_4111249
_publ_section_title
;
 Carbon-Oxygen Bond Cleavage with \h9,\h5-Bis(indenyl)zirconium Sandwich
 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16600
_journal_page_last               16612
_journal_paper_doi               10.1021/ja065456g
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C32 H50 Si4 Zr'
_chemical_formula_weight         638.30
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.617(4)
_cell_angle_beta                 98.394(4)
_cell_angle_gamma                90.769(4)
_cell_formula_units_Z            4
_cell_length_a                   10.3139(18)
_cell_length_b                   17.875(3)
_cell_length_c                   19.132(3)
_cell_measurement_temperature    173(2)
_cell_volume                     3488.8(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0548
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32707
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.471
_exptl_absorpt_correction_T_max  0.9768
_exptl_absorpt_correction_T_min  0.8525
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.019
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1022
_refine_ls_number_reflns         17015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.156
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.3212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1054
_reflns_number_gt                11867
_reflns_number_total             17015
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja065456gsi20060728_040233.cif
_cod_data_source_block           cb29
_cod_original_cell_volume        3488.9(11)
_cod_database_code               4111249