Nucleophilic Character of a Charge Neutral, High Oxidation State d0 Zirconium Trimethylenemethane Complex
Denis A. Kissounko; Lawrence R. Sita; Journal of the American Chemical Society 126 (2004) 5946–5947; doi:10.1021/ja0493897

data_4112566
_publ_section_title
;
 Nucleophilic Character of a Charge Neutral, High Oxidation State d0
 Zirconium Trimethylenemethane Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5946
_journal_page_last               5947
_journal_paper_doi               10.1021/ja0493897
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'C24 H41 F3 N2 O3 S Zr'
_chemical_formula_sum            'C24 H41 F3 N2 O3 S Zr'
_chemical_formula_weight         585.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 112.7720(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.3351(8)
_cell_length_b                   18.4480(8)
_cell_length_c                   16.6791(7)
_cell_measurement_reflns_used    8626
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      53.583
_cell_measurement_theta_min      4.570
_cell_volume                     5485.6(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      163(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0597
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            91379
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.14
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.524
_exptl_absorpt_correction_T_max  0.9524
_exptl_absorpt_correction_T_min  0.8145
_exptl_absorpt_correction_type   'SADABS, multi-scan'
_exptl_absorpt_process_details   'Blessing,R.H.(1995).Acta Cryst.,A51,33-38.'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_meas      0
_exptl_crystal_description       Rod
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.887
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     975
_refine_ls_number_reflns         12596
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+4.2205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0966
_reflns_number_gt                8779
_reflns_number_total             12596
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0493897si20040203_025113.cif
_cod_data_source_block           979ff1
_cod_database_code               4112566