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_4516063
_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         'C40 H66 N3 Nb O'
_chemical_formula_sum            'C40 H66 N3 Nb O'
_chemical_formula_weight         697.88
_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                89.366(3)
_cell_angle_beta                 88.443(3)
_cell_angle_gamma                75.219(3)
_cell_formula_units_Z            4
_cell_length_a                   12.5502(4)
_cell_length_b                   14.0719(5)
_cell_length_c                   23.5634(9)
_cell_measurement_reflns_used    15887
_cell_measurement_temperature    93
_cell_measurement_theta_max      28.61
_cell_measurement_theta_min      2.40
_cell_volume                     4022.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0777
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            67935
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.518
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.330
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.510
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1504.00
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.064
_refine_diff_density_max         4.07
_refine_diff_density_min         -2.36
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.251
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     811
_refine_ls_number_reflns         17259
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1584
_refine_ls_R_factor_gt           0.1366
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+93.3720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3099
_refine_ls_wR_factor_ref         0.3184
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13682
_reflns_number_total             17259
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ao8b01065_si_002.cif
_cod_data_source_block           complex4b
_cod_depositor_comments
;

2020-05-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C80 H132 N6 Nb2 O2'
_cod_original_formula_weight         1395.77
_cod_original_formula_moiety         'C80 H132 N6 Nb2 O2'
_cod_original_formula_units_Z            2
_cod_database_code               4516063
_shelx_res_checksum              1849
_shelx_hkl_checksum              58487