Synthesis and reactivity of cationic niobium and tantalum methyl complexes supported by imido and β-diketiminato ligands.
Tomson, Neil C.; Arnold, John; Bergman, Robert G.; Dalton transactions (Cambridge, England : 2003) 40 (2011) 7718–7729; doi:10.1039/c1dt10202h

data_7016089
_publ_section_title
;
 Synthesis and reactivity of cationic niobium and tantalum methyl
 complexes supported by imido and \b-diketiminato ligands.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7718
_journal_page_last               7729
_journal_paper_doi               10.1039/c1dt10202h
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C34.86 H55.58 Cl0.14 N3 Ta'
_chemical_formula_sum            'C34.86 H55.58 Cl0.14 N3 Ta'
_chemical_formula_weight         702.65
_chemical_name_systematic
;
?
;
_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                 93.375(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4872(15)
_cell_length_b                   13.1367(19)
_cell_length_c                   24.997(4)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    147(2)
_cell_measurement_theta_max      56.574
_cell_measurement_theta_min      4.499
_cell_volume                     3437.8(9)
_computing_cell_refinement       'Bruker APEX2 v. 2009.1'
_computing_data_collection       'Bruker APEX2 v. 2009.1'
_computing_data_reduction        'Bruker APEX2 v. 2009.1'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      147(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       '\f and \w 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  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            21789
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    3.301
_exptl_absorpt_correction_T_max  0.6202
_exptl_absorpt_correction_T_min  0.4088
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1508
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.406
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         8300
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0320P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0803
_reflns_number_gt                6457
_reflns_number_total             8300
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10202h.txt
_cod_data_source_block           neils
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7016089