Enantioselective Synthesis of ansa-Zirconocenes
Matthew D. LoCoco; Richard F. Jordan; Journal of the American Chemical Society 126 (2004) 13918–13919; doi:10.1021/ja045245g

data_4113105
_publ_section_title
;
 Enantioselective Synthesis of ansa-Zirconocenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13918
_journal_page_last               13919
_journal_paper_doi               10.1021/ja045245g
_journal_volume                  126
_journal_year                    2004
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(C27 H30 N2 Zr), 1.5(C6 H6)'
_chemical_formula_sum            'C63 H69 N4 Zr2'
_chemical_formula_weight         1064.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 99.105(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.777(12)
_cell_length_b                   8.697(4)
_cell_length_c                   22.295(10)
_cell_measurement_temperature    138(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.21
_cell_volume                     5127(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      138(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       '\W 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  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20652
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.450
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS, SHELXTL (version 5.1) program library 
(G. Sheldrick, Bruker Analytical X-ray Systems, Madison, WI)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_F_000             2220
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.605
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         9034
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.605
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.062
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0860P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0673
_reflns_number_gt                8571
_reflns_number_total             9034
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja045245gsi20040902_010007.cif
_cod_data_source_block           matt08s
_cod_database_code               4113105