A New Perfluorinated F21-Tp Scorpionate Ligand: Enhanced Alkane Functionalization by Carbene Insertion with (F21-Tp)M Catalysts (M = Cu, Ag)
Despagnet-Ayoub, Emmanuelle; Jacob, Kane; Vendier, Laure; Etienne, Michel; Álvarez, Eleuterio; Caballero, Ana; Díaz-Requejo, M. Mar; Pérez, Pedro J.; Organometallics 27 (2008) 4779–; doi:10.1021/om800531a

data_4072028
_publ_section_title
;
 A New Perfluorinated F21-Tp Scorpionate Ligand: Enhanced Alkane
 Functionalization by Carbene Insertion with (F21-Tp)M Catalysts (M = Cu,
 Ag)
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4779
_journal_paper_doi               10.1021/om800531a
_journal_volume                  27
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C25 H1 B1 Cu1 F21 N6 O1'
_chemical_formula_sum            'C25 H B Cu F21 N6 O'
_chemical_formula_weight         874.67
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 94.000(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4150(6)
_cell_length_b                   11.6353(8)
_cell_length_c                   28.0159(16)
_cell_measurement_reflns_used    4430
_cell_measurement_temperature    180
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.8
_cell_measurement_wavelength     0.71073
_cell_volume                     3061.6(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       \w-\f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            24837
_diffrn_reflns_theta_full        24.95
_diffrn_reflns_theta_max         24.95
_diffrn_reflns_theta_min         1.46
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.898
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         5339
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+0.7782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1161
_reflns_number_gt                3676
_reflns_number_total             5339
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om800531a_si_004.cif
_cod_data_source_block           3
_cod_database_code               4072028