ansa-Zirconocene Ester Enolates: Synthesis, Structure, Reaction with Organo-Lewis Acids, and Application to Polymerization of Methacrylates
Andrew D. Bolig; Eugene Y.-X. Chen; Journal of the American Chemical Society 126 (2004) 4897–4906; doi:10.1021/ja031558k

data_4112438
_publ_section_title
;
 ansa-Zirconocene Ester Enolates: Synthesis, Structure, Reaction with
 Organo-Lewis Acids, and Application to Polymerization of Methacrylates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4897
_journal_page_last               4906
_journal_paper_doi               10.1021/ja031558k
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C34 H42 O4 Zr'
_chemical_formula_weight         605.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.308(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.52(2)
_cell_length_b                   11.188(11)
_cell_length_c                   13.016(12)
_cell_measurement_temperature    173(2)
_cell_volume                     3101(5)
_computing_cell_refinement       'Bruker SMART'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.1084
_diffrn_reflns_av_sigmaI/netI    0.1151
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9255
_diffrn_reflns_theta_full        23.38
_diffrn_reflns_theta_max         23.38
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.389
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_meas      0
_exptl_crystal_description       cubes
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.955
_refine_diff_density_min         -1.016
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.0001(4)
_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   1.133
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0721
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+4.9439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1659
_refine_ls_wR_factor_ref         0.1741
_reflns_number_gt                1941
_reflns_number_total             2259
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja031558ksi20040208_014057.cif
_cod_data_source_block           complex2
_cod_database_code               4112438