Formation of a Dicationic Yttrium η2-Pyridyl Complex from an Yttrium Methyl Dication by C−H Activation of Pyridine
Arndt, Stefan; Elvidge, Benjamin R.; Zeimentz, Peter M.; Spaniol, Thomas P.; Okuda, Jun; Organometallics 25 (2006) 793–; doi:10.1021/om0509140

data_4074818
_publ_section_title
;
 Formation of a Dicationic Yttrium \h2-Pyridyl Complex from an Yttrium
 Methyl Dication by C&#x2212;H Activation of Pyridine
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              793
_journal_paper_doi               10.1021/om0509140
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C88 H79 B2 N8 Y'
_chemical_formula_weight         1359.18
_chemical_name_systematic
;
 ?
;
_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                   13.9108(5)
_cell_length_b                   22.5453(6)
_cell_length_c                   23.4052(7)
_cell_measurement_reflns_used    6579
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      20.64
_cell_measurement_theta_min      2.27
_cell_volume                     7340.4(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0922
_diffrn_reflns_av_sigmaI/netI    0.0837
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            136513
_diffrn_reflns_theta_full        27.64
_diffrn_reflns_theta_max         27.64
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.846
_exptl_absorpt_correction_T_max  0.8163
_exptl_absorpt_correction_T_min  0.7853
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2847
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.021(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     892
_refine_ls_number_reflns         17052
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0651P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1339
_reflns_number_gt                12766
_reflns_number_total             17052
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0509140si20051021_043144.cif
_cod_data_source_block           sa34
_cod_database_code               4074818