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_4113189
_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            'C106 H102 N4 Si2 Zr2'
_chemical_formula_weight         1670.5
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.99(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   43.912(7)
_cell_length_b                   16.786(3)
_cell_length_c                   11.467(2)
_cell_measurement_temperature    210(2)
_cell_volume                     8390(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            17560
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.330
_exptl_absorpt_correction_T_max  0.9386
_exptl_absorpt_correction_T_min  0.8265
_exptl_absorpt_correction_type   'psi scans'
_exptl_absorpt_process_details   'SHELXTL(Version 5.1)'
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_F_000             3496
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.036
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1039
_refine_ls_number_reflns         14477
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+14.8753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1220
_reflns_number_gt                9858
_reflns_number_total             14477
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0466292Bsi20040908_120805.cif
_cod_data_source_block           jor81
_cod_database_code               4113189