Stabilizing Zr and Ti Cations by Interaction With a Ferrocenyl Fragment
Alberto Ramos; Edwin Otten; Douglas W. Stephan; Journal of the American Chemical Society 131 (2009) 15610–15611; doi:10.1021/ja9077446

data_4105275
_publ_section_title
;
 Stabilizing Zr and Ti Cations by Interaction With a Ferrocenyl Fragment
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15610
_journal_page_last               15611
_journal_paper_doi               10.1021/ja9077446
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C39 H22 B F15 Fe Zr'
_chemical_formula_weight         933.45
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1770(11)
_cell_length_b                   15.8640(14)
_cell_length_c                   16.2706(14)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     3401.2(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            73813
_diffrn_reflns_theta_full        38.07
_diffrn_reflns_theta_max         38.07
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.847
_exptl_absorpt_correction_T_max  0.7475
_exptl_absorpt_correction_T_min  0.6774
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.004(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         18081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0331P)^2^+0.3329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0714
_reflns_number_gt                15672
_reflns_number_total             18081
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9077446_si_002_1.cif
_cod_data_source_block           '[Cp2Zr(C5H4)FeCp][MeB(C6F5)3]'
_cod_database_code               4105275