Synthesis of (Arylmido)niobium(V) Complexes Containing Ketimide, Phenoxide Ligands, and Some Reactions with Phenols and Alcohols.
Srisupap, Natta; Wised, Kritdikul; Tsutsumi, Ken; Nomura, Kotohiro; ACS omega 3 (2018) 6166–6181; doi:10.1021/acsomega.8b01065

data_4516064
_publ_section_title
;
 Synthesis of (Arylmido)niobium(V) Complexes Containing Ketimide,
 Phenoxide Ligands, and Some Reactions with Phenols and Alcohols.
;
_journal_issue                   6
_journal_name_full               'ACS omega'
_journal_page_first              6166
_journal_page_last               6181
_journal_paper_doi               10.1021/acsomega.8b01065
_journal_volume                  3
_journal_year                    2018
_chemical_formula_moiety         'C45 H55 F15 N3 Nb O3'
_chemical_formula_sum            'C45 H55 F15 N3 Nb O3'
_chemical_formula_weight         1063.83
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                86.879(3)
_cell_angle_beta                 81.525(3)
_cell_angle_gamma                77.672(3)
_cell_formula_units_Z            2
_cell_length_a                   11.3778(5)
_cell_length_b                   12.9307(5)
_cell_length_c                   18.9950(6)
_cell_measurement_reflns_used    12763
_cell_measurement_temperature    93
_cell_measurement_theta_max      30.44
_cell_measurement_theta_min      2.32
_cell_volume                     2699.58(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2.5'
_computing_publication_material  'CrystalStructure 4.2.5 (Rigaku, 2017)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22400
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.648
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.312
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1092.00
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.253
_exptl_crystal_size_min          0.238
_refine_diff_density_max         1.28
_refine_diff_density_min         -1.27
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     652
_refine_ls_number_reflns         11596
_refine_ls_number_restraints     120
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0643
_refine_ls_shift/su_max          0.032
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0883P)^2^+11.0188P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1972
_refine_ls_wR_factor_ref         0.2013
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9893
_reflns_number_total             11596
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ao8b01065_si_002.cif
_cod_data_source_block           7
_cod_database_code               4516064
_shelx_res_checksum              94991
_shelx_hkl_checksum              86331
_shelx_fab_checksum              35065