A New ONO3-Trianionic Pincer-Type Ligand for Generating Highly Nucleophilic Metal-Carbon Multiple Bonds
Matthew E. O'Reilly; Ion Ghiviriga; Khalil A. Abboud; Adam S. Veige; Journal of the American Chemical Society 134 (2012) 11185–11195; doi:10.1021/ja302222s

data_4118214
_publ_section_title
;
 A New ONO3-Trianionic Pincer-Type Ligand for Generating Highly
 Nucleophilic Metal-Carbon Multiple Bonds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11185
_journal_page_last               11195
_journal_paper_doi               10.1021/ja302222s
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C27 H26.94 Br0.03 F12 N O3 W'
_chemical_formula_weight         827.68
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_audit_update_record
;
2011-05-03 # Formatted by publCIF
;
_cell_angle_alpha                86.891(2)
_cell_angle_beta                 82.183(2)
_cell_angle_gamma                70.699(2)
_cell_formula_units_Z            2
_cell_length_a                   8.5483(3)
_cell_length_b                   9.4574(3)
_cell_length_c                   19.5076(6)
_cell_measurement_reflns_used    9851
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     1474.54(9)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL (Bruker, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'SMART CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28207
_diffrn_reflns_theta_full        25.48
_diffrn_reflns_theta_max         25.48
_diffrn_reflns_theta_min         1.05
_diffrn_standards_decay_%        1
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.064
_exptl_absorpt_correction_T_max  0.6607
_exptl_absorpt_correction_T_min  0.5304
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL  v6.14 (Bruker 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.864
_exptl_crystal_description       irregular
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.198
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         5441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0173P)^2^+0.9282P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0476
_refine_ls_wR_factor_ref         0.0503
_reflns_number_gt                4758
_reflns_number_total             5441
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja302222s_si_001_2.cif
_cod_data_source_block           orei24
_cod_original_cell_volume        1474.54(8)
_cod_database_code               4118214