Regioselective C-H Activation and Sequential C-C and C-O Bond Formation Reactions of Aryl Ketones Promoted by an Yttrium Carbene
David P. Mills; Lyndsay Soutar; William Lewis; Alexander J. Blake; Stephen T. Liddle; Journal of the American Chemical Society 132 (2010) 14379–14381; doi:10.1021/ja107958u

data_4103336
_publ_section_title
;
 Regioselective C-H Activation and Sequential C-C and C-O Bond Formation
 Reactions of Aryl Ketones Promoted by an Yttrium Carbene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14379
_journal_page_last               14381
_journal_paper_doi               10.1021/ja107958u
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C57 H58 I N2 O2 P2 Si2 Y, 0.5(C4 H8 O)'
_chemical_formula_sum            'C59 H62 I N2 O2.5 P2 Si2 Y'
_chemical_formula_weight         1173.04
_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, Me from difmap'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha                90.00
_cell_angle_beta                 111.670(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.828(2)
_cell_length_b                   10.4486(11)
_cell_length_c                   26.112(3)
_cell_measurement_reflns_used    6170
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      2.20
_cell_volume                     5788.1(10)
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction
'Bruker SAINT; Bruker SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material
'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_av_sigmaI/netI    0.070
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            22923
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.680
_exptl_absorpt_correction_T_max  0.70
_exptl_absorpt_correction_T_min  0.49
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.16
_refine_diff_density_min         -1.49
_refine_diff_density_rms         0.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.97
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     610
_refine_ls_number_reflns         10136
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.97
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0776P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.124
_refine_ls_wR_factor_ref         0.130
_reflns_number_gt                7644
_reflns_number_total             10136
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja107958u_si_004.cif
_cod_data_source_block           ypnphi
_cod_original_cell_volume        5788.1(11)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C59 H62 I N2 O2.50 P2 Si2 Y'
_cod_database_code               4103336