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_7014636
_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         'C59.50 H87.50 Cl3 N Nb O3'
_chemical_formula_sum            'C59.5 H87.5 Cl3 N Nb O3'
_chemical_formula_weight         1064.12
_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
_cell_angle_alpha                94.951(6)
_cell_angle_beta                 99.947(5)
_cell_angle_gamma                97.388(7)
_cell_formula_units_Z            4
_cell_length_a                   13.987(6)
_cell_length_b                   20.447(8)
_cell_length_c                   21.538(9)
_cell_measurement_reflns_used    14703
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.00
_cell_volume                     5979(4)
_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 0.941
_diffrn_measured_fraction_theta_max 0.941
_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  0.0449
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            45362
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.376
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2270.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.420
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1201
_refine_ls_number_reflns         24585
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0658
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0518P)^2^+11.7241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1520
_reflns_number_gt                18783
_reflns_number_total             24591
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            C0DT01022G.TXT
_cod_data_source_block           '_O3NbCl3-syn-Complex-3-syn'
_cod_original_cell_volume        5980(4)
_cod_original_formula_sum        'C59.50 H87.50 Cl3 N Nb O3'
_cod_database_code               7014636