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_4105277
_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            'C43.5 H32.25 B Br0.25 F15 Fe P Zr'
_chemical_formula_weight         1048.77
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                110.254(2)
_cell_angle_beta                 97.413(2)
_cell_angle_gamma                91.311(2)
_cell_formula_units_Z            4
_cell_length_a                   12.7013(6)
_cell_length_b                   15.4895(8)
_cell_length_c                   22.0666(11)
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     4028.2(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            101607
_diffrn_reflns_theta_full        31.72
_diffrn_reflns_theta_max         31.72
_diffrn_reflns_theta_min         0.99
_exptl_absorpt_coefficient_mu    1.010
_exptl_absorpt_correction_T_max  0.9058
_exptl_absorpt_correction_T_min  0.7515
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_F_000             2092
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.837
_refine_diff_density_min         -1.020
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1162
_refine_ls_number_reflns         27023
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+1.8288P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0883
_reflns_number_gt                20403
_reflns_number_total             27023
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9077446_si_002_3.cif
_cod_data_source_block           '[Cp2Zr(C5H4)FeCp(PMe3)][MeB(C6F5)3](C6H5Br)'
_cod_original_cell_volume        4028.2(3)
_cod_original_formula_sum        'C43.50 H32.25 B Br0.25 F15 Fe P Zr'
_cod_database_code               4105277