Synthesis and reactivity of niobium complexes having a tripodal triaryloxide ligand in bidentate, tridentate, and tetradentate coordination modes.
Akagi, Fumio; Ishida, Yutaka; Matsuo, Tsukasa; Kawaguchi, Hiroyuki; Dalton transactions (Cambridge, England : 2003) 40 (2011) 2375–2382; doi:10.1039/c0dt01022g

data_7014638
_publ_section_title
;
 Synthesis and reactivity of niobium complexes having a tripodal
 triaryloxide ligand in bidentate, tridentate, and tetradentate
 coordination modes.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2375
_journal_page_last               2382
_journal_paper_doi               10.1039/c0dt01022g
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C50 H67 Nb O3'
_chemical_formula_sum            'C50 H67 Nb O3'
_chemical_formula_weight         808.98
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 110.455(5)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   14.679(5)
_cell_length_b                   11.916(4)
_cell_length_c                   27.664(9)
_cell_measurement_reflns_used    11763
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.04
_cell_volume                     4534(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            35050
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1728.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.130
_refine_diff_density_min         -0.580
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     481
_refine_ls_number_reflns         10347
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0684
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0894P)^2^+5.7055P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1779
_reflns_number_gt                8895
_reflns_number_total             10347
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            C0DT01022G.TXT
_cod_data_source_block           '_O3CNbBn-Complex-5'
_cod_database_code               7014638