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_4080485
_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         'C39 H51 N4 O Si Y'
_chemical_formula_sum            'C39 H51 N4 O Si Y'
_chemical_formula_weight         708.84
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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      2.4
_audit_creation_date             2012-03-21T14:52:45-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 101.108(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.061(3)
_cell_length_b                   18.161(3)
_cell_length_c                   31.122(6)
_cell_measurement_reflns_used    6840
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      20.14
_cell_measurement_theta_min      2.44
_cell_measurement_wavelength     0.71073
_cell_volume                     7798(3)
_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      250(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.1059
_diffrn_reflns_av_unetI/netI     0.155
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            68336
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.42
_exptl_absorpt_coefficient_mu    1.559
_exptl_absorpt_correction_T_max  0.804
_exptl_absorpt_correction_T_min  0.691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2992
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.98
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     835
_refine_ls_number_reflns         17751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.98
_refine_ls_R_factor_all          0.1964
_refine_ls_R_factor_gt           0.0622
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.149
_reflns_number_gt                7399
_reflns_number_total             17751
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400027d_si_002.cif
_cod_data_source_block           2a_prim
_cod_depositor_comments
;

2026-05-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C78 H102 N8 O2 Si2 Y2'
_cod_original_formula_weight         1417.68
_cod_original_formula_moiety         '2(C39 H51 N4 O Si Y)'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               4080485