Chelate-Controlled Synthesis of Racemic ansa-Zirconocenes
Matthew D. LoCoco; Xingwang Zhang; Richard F. Jordan; Journal of the American Chemical Society 126 (2004) 15231–15244; doi:10.1021/ja046629+

data_4113193
_publ_section_title
;
 Chelate-Controlled Synthesis of Racemic ansa-Zirconocenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15231
_journal_page_last               15244
_journal_paper_doi               10.1021/ja046629+
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C45 H42 N2 Si Zr'
_chemical_formula_weight         730.12
_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                93.5030(10)
_cell_angle_beta                 97.2190(10)
_cell_angle_gamma                107.1250(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3355(6)
_cell_length_b                   12.1037(7)
_cell_length_c                   14.8777(8)
_cell_measurement_temperature    173(2)
_cell_volume                     1755.08(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      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0934
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7121
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.383
_exptl_absorpt_correction_T_max  0.9627
_exptl_absorpt_correction_T_min  0.9448
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_description       Fragment
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         7121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0230P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0814
_reflns_number_gt                4867
_reflns_number_total             7121
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0466292Bsi20040908_120936.cif
_cod_data_source_block           jor27
_cod_database_code               4113193