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_4113195
_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            'C22 H32 Cl2 N2 O2 Zr'
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_chemical_name_systematic
; 
 ? 
;
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_formula_units_Z            8
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_cell_length_b                   10.855(2)
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_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      15.7
_cell_measurement_theta_min      12.6
_cell_volume                     4809.3(19)
_computing_cell_refinement       'CAD-4 Manual (Enraf-Nonius,1977)'
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_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    'SHELXTL v5.0 (Sheldrick, 1995)'
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_computing_structure_refinement  'SHELXTL v5.0 (Sheldrick, 1995)'
_computing_structure_solution    'SHELXTL v5.0 (Sheldrick, 1995)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measured_fraction_theta_max 1.0
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       '\q-2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
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_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    0.699
_exptl_absorpt_correction_T_max  0.8541
_exptl_absorpt_correction_T_min  0.8322
_exptl_absorpt_correction_type   'psi scans'
_exptl_absorpt_process_details
; 
Blessing,R. H. Acta Cryst. 1995, A51, 33-38 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       prism
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_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.277
_exptl_crystal_size_min          0.229
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_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.065
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         2104
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.065
_refine_ls_restrained_S_obs      1.073
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0230
_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^)+(0.0363P)^2^+1.7550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.0580
_reflns_number_gt                1964
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_reflns_threshold_expression     >2sigma(I)
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_cod_data_source_block           jor98_3
_cod_original_cell_volume        4809(2)
_cod_database_code               4113195