Tandem C(sp(2))-OMe Activation/C(sp(2))-C(sp(2)) Coupling in Early Transition-Metal Complexes: Aromatic C-O Activation beyond Late Transition Metals.
Radkov, Vasily; Roisnel, Thierry; Trifonov, Alexander; Carpentier, Jean-François; Kirillov, Evgueni; Journal of the American Chemical Society 138 (2016) 4350–4353; doi:10.1021/jacs.6b01877

data_4130282
_publ_section_title
;
 Tandem C(sp(2))-OMe Activation/C(sp(2))-C(sp(2)) Coupling in Early
 Transition-Metal Complexes: Aromatic C-O Activation beyond Late
 Transition Metals.
;
_journal_issue                   13
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4350
_journal_page_last               4353
_journal_paper_doi               10.1021/jacs.6b01877
_journal_volume                  138
_journal_year                    2016
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C60 H55 F6 N8 O2 Sc, 2.5(C6 H6)'
_chemical_formula_sum            'C75 H70 F6 N8 O2 Sc'
_chemical_formula_weight         1274.35
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2014-06-05T14:24:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                73.837(6)
_cell_angle_beta                 84.453(6)
_cell_angle_gamma                64.670(6)
_cell_formula_units_Z            2
_cell_length_a                   11.8165(18)
_cell_length_b                   13.720(2)
_cell_length_c                   22.645(4)
_cell_measurement_reflns_used    5686
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.05
_cell_measurement_theta_min      2.33
_cell_measurement_wavelength     0.71073
_cell_volume                     3186.1(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, 2012),
           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 0.976
_diffrn_measured_fraction_theta_max 0.939
_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  0.0901
_diffrn_reflns_av_unetI/netI     0.1636
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            32971
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    0.188
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             1334
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.0095(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         13737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1975
_refine_ls_R_factor_gt           0.1009
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1123P)^2^+10.3599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2576
_refine_ls_wR_factor_ref         0.3056
_reflns_number_gt                6622
_reflns_number_total             13737
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b01877_si_002.cif
_cod_data_source_block           1-Sc
_cod_database_code               4130282