Synthesis and Reactivity of Tantalum Complexes Supported by the Pincer Ligand 2,6-Pyridinedicarboxylate. Preparation of an Unprecedented Water-Soluble Iminoacyl Complex
Conde, Ana; Fandos, Rosa; Otero, Antonio; Rodríguez, Ana; Organometallics 28 (2009) 5505–; doi:10.1021/om900643c

data_4070192
_publ_section_title
;
 Synthesis and Reactivity of Tantalum Complexes Supported by the Pincer
 Ligand 2,6-Pyridinedicarboxylate. Preparation of an Unprecedented
 Water-Soluble Iminoacyl Complex
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              5505
_journal_paper_doi               10.1021/om900643c
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C37 H21 B F18 N O7 S Ta, 0.5(C2 H4 Cl4)'
_chemical_formula_sum            'C38 H23 B Cl2 F18 N O7 S Ta'
_chemical_formula_weight         1242.29
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.912(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2470(12)
_cell_length_b                   11.809(3)
_cell_length_c                   32.3160(18)
_cell_measurement_reflns_used    1012
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      16.99
_cell_measurement_theta_min      2.45
_cell_volume                     4251.2(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT, SADABS, XPREP'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0909
_diffrn_reflns_av_sigmaI/netI    0.1253
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            26902
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    2.890
_exptl_absorpt_correction_T_max  0.6097
_exptl_absorpt_correction_T_min  0.4489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.941
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.253
_refine_diff_density_min         -1.163
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         7479
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.078
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0835
_reflns_number_gt                3233
_reflns_number_total             7479
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900643c_si_001.cif
_cod_data_source_block           6
_cod_original_cell_volume        4251.2(13)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4070192