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_4516062
_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         'C39 H64 Cl2 N3 Nb O'
_chemical_formula_sum            'C39 H64 Cl2 N3 Nb O'
_chemical_formula_weight         754.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        '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                 93.169(5)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   15.469(3)
_cell_length_b                   10.6814(19)
_cell_length_c                   24.897(4)
_cell_measurement_reflns_used    8592
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.00
_cell_volume                     4107.5(13)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b45'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b45'
_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 5.814
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.932
_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  0.0646
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            60816
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.540
_diffrn_reflns_theta_min         3.028
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.454
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1608.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.85
_refine_diff_density_min         -0.68
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     415
_refine_ls_number_reflns         8829
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0505P)^2^+6.9906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1291
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6583
_reflns_number_total             8829
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ao8b01065_si_002.cif
_cod_data_source_block           4a
_cod_database_code               4516062
_shelx_res_checksum              21596
_shelx_hkl_checksum              91299