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_7016087
_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         'C66 H73 B F20 N3 Nb O2'
_chemical_formula_sum            'C66 H73 B F20 N3 Nb O2'
_chemical_formula_weight         1423.99
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                114.348(2)
_cell_angle_beta                 102.282(3)
_cell_angle_gamma                91.108(3)
_cell_formula_units_Z            2
_cell_length_a                   13.616(3)
_cell_length_b                   16.444(3)
_cell_length_c                   17.040(3)
_cell_measurement_reflns_used    2444
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      42.695
_cell_measurement_theta_min      6.860
_cell_volume                     3371.7(11)
_computing_cell_refinement       'Bruker SAINT v7.07'
_computing_data_collection       'Bruker SMART v5.054d'
_computing_data_reduction        'Bruker SAINT v7.07'
_computing_molecular_graphics    'Bruker-AXS XP v.6'
_computing_publication_material  'Bruker-AXS XP v.6'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'SMART 1000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0734
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12998
_diffrn_reflns_theta_full        21.72
_diffrn_reflns_theta_max         21.72
_diffrn_reflns_theta_min         3.43
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.815713
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.885
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         7758
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0695P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1315
_reflns_number_gt                5193
_reflns_number_total             7758
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10202h.txt
_cod_data_source_block           n5c69txs
_cod_original_cell_volume        3371.6(11)
_cod_database_code               7016087