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_4113191
_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            'C44 H42 N2 Si Zr'
_chemical_formula_weight         718.11
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 99.97(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.165(8)
_cell_length_b                   15.453(4)
_cell_length_c                   11.026(3)
_cell_measurement_reflns_used    21
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      11.3
_cell_volume                     3551.7(19)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       'theta-2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7471
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        2.7
_diffrn_standards_interval_time  '2 hr'
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    0.377
_exptl_absorpt_correction_T_max  0.9095
_exptl_absorpt_correction_T_min  0.8295
_exptl_absorpt_correction_type   'psi scans'
_exptl_absorpt_process_details
; 
Blessing,R. H. Acta Cryst. 1995, A51, 33-38 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       prism
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.639
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.100
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         6110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_restrained_S_obs      1.058
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0545
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          -0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0815P)^2^+5.5990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1636
_refine_ls_wR_factor_ref         0.1334
_reflns_number_gt                4492
_reflns_number_total             6110
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0466292Bsi20040908_120851.cif
_cod_data_source_block           JOR97_F
_cod_original_cell_volume        3552(2)
_cod_database_code               4113191