Reduction of ((t)BuN═)NbCl3(py)2 in a Salt-Free Manner for Generating Nb(IV) Dinuclear Complexes and Their Reactivity toward Benzo[c]cinnoline.
Saito, Teruhiko; Nishiyama, Haruka; Kawakita, Kento; Nechayev, Michael; Kriegel, Benjamin; Tsurugi, Hayato; Arnold, John; Mashima, Kazushi; Inorganic chemistry 54 (2015) 6004–6009; doi:10.1021/acs.inorgchem.5b00812

data_1520056
_publ_section_title
;
 Reduction of ((t)BuN&#x2550;)NbCl3(py)2 in a Salt-Free Manner for
 Generating Nb(IV) Dinuclear Complexes and Their Reactivity toward
 Benzo[c]cinnoline.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6004
_journal_page_last               6009
_journal_paper_doi               10.1021/acs.inorgchem.5b00812
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C31.50 H48 Cl4 N6 Nb2 O2'
_chemical_formula_sum            'C31.5 H48 Cl4 N6 Nb2 O2'
_chemical_formula_weight         870.38
_chemical_name_common            Complex6
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.009(4)
_cell_angle_beta                 92.687(4)
_cell_angle_gamma                92.922(4)
_cell_formula_units_Z            2
_cell_length_a                   8.4679(5)
_cell_length_b                   15.5173(9)
_cell_length_c                   15.6028(9)
_cell_measurement_reflns_used    9404
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.73
_cell_measurement_theta_min      2.61
_cell_volume                     2045.3(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Yadokari-XG 2009'
_computing_publication_material  'Yadokari-XG 2009'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0981
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28328
_diffrn_reflns_theta_full        29.82
_diffrn_reflns_theta_max         29.82
_diffrn_reflns_theta_min         1.85
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.855
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             890
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.078
_refine_diff_density_min         -1.325
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         11655
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1080
_refine_ls_R_factor_gt           0.0627
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1603
_refine_ls_wR_factor_ref         0.1894
_reflns_number_gt                7659
_reflns_number_total             11655
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00812_si_003.cif
_cod_data_source_block           Complex6
_cod_depositor_comments
'Adding full bibliography for 1520054--1520057.cif.'
_cod_original_formula_sum        'C31.50 H48 Cl4 N6 Nb2 O2'
_cod_database_code               1520056