Alkylyttrium Complexes of Amidine‒Amidopyridinate Ligands. Intramolecular C(sp3)‒H Activation and Reactivity Studies
Rad’kov, Vasily; Dorcet, Vincent; Carpentier, Jean-François; Trifonov, Alexander; Kirillov, Evgeny; Organometallics 32 (2013) 1517–; doi:10.1021/om400027d

data_4080487
_publ_section_title
;
 Alkylyttrium Complexes of Amidine--Amidopyridinate Ligands.
 Intramolecular C(sp3)--H Activation and Reactivity Studies
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1517
_journal_paper_doi               10.1021/om400027d
_journal_volume                  32
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C70 H86 N8 O2 Si2 Y2, 2(C7 H8)'
_chemical_formula_sum            'C84 H102 N8 O2 Si2 Y2'
_chemical_formula_weight         1489.74
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2012-01-20T13:39:19-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 121.401(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.1225(15)
_cell_length_b                   14.6664(7)
_cell_length_c                   29.2667(17)
_cell_measurement_reflns_used    7031
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.14
_cell_measurement_theta_min      2.52
_cell_measurement_wavelength     0.71073
_cell_volume                     8837.8(9)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
;
           WinGX publication routines (Farrugia, 1999),
           CRYSCAL (T. Roisnel, local program)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.065
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            40414
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    1.379
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.12
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
;
_refine_diff_density_max         0.72
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         10106
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.076
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1241
_reflns_number_gt                7125
_reflns_number_total             10106
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400027d_si_002.cif
_cod_data_source_block           7_C7H8
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4080487