Influence of Hydrogen Bonds on the Stability of Some Cationic Monoaminocarbene Tantalum Complexes Containing Tridentate Bis(phenolato) [OSO]-Type Ligands
Fandos, Rosa; Fernández-Gallardo, Jacob; Otero, Antonio; Rodríguez, Ana; Ruiz, María José; Organometallics 29 (2010) 5834–; doi:10.1021/om100541g

data_4066604
_publ_section_title
;
 Influence of Hydrogen Bonds on the Stability of Some Cationic
 Monoaminocarbene Tantalum Complexes Containing Tridentate Bis(phenolato)
 [OSO]-Type Ligands
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5834
_journal_paper_doi               10.1021/om100541g
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         '2(C32 H33 Cl4 N O3 S Ta), C H2 Cl2, 2(Cl)'
_chemical_formula_sum            'C65 H68 Cl12 N2 O6 S2 Ta2'
_chemical_formula_weight         1824.65
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 107.246(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.107(3)
_cell_length_b                   17.260(3)
_cell_length_c                   15.701(3)
_cell_measurement_reflns_used    826
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      16.641
_cell_measurement_theta_min      2.359
_cell_volume                     3651.1(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 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '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  0.1262
_diffrn_reflns_av_sigmaI/netI    0.1775
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24828
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    3.540
_exptl_absorpt_correction_T_max  0.7412
_exptl_absorpt_correction_T_min  0.5844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1804
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.041
_refine_diff_density_min         -1.513
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.905
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         8530
_refine_ls_number_restraints     274
_refine_ls_restrained_S_all      0.893
_refine_ls_R_factor_all          0.1447
_refine_ls_R_factor_gt           0.0658
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0651P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1329
_refine_ls_wR_factor_ref         0.1648
_reflns_number_gt                4207
_reflns_number_total             8530
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100541g_si_001.cif
_cod_data_source_block           8
_cod_original_cell_volume        3651.3(12)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4066604