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_1520055
_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         'C23 H33 Cl4 N5 Nb2'
_chemical_formula_sum            'C23 H33 Cl4 N5 Nb2'
_chemical_formula_weight         707.16
_chemical_name_common            Complex4
_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                87.369(6)
_cell_angle_beta                 83.921(6)
_cell_angle_gamma                77.279(6)
_cell_formula_units_Z            2
_cell_length_a                   8.5962(12)
_cell_length_b                   11.0422(16)
_cell_length_c                   15.754(2)
_cell_measurement_reflns_used    9724
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.27
_cell_volume                     1450.1(3)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0145
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            40131
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.89
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.180
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         5290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.901
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0208
_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          0.0959
_refine_ls_wR_factor_ref         0.0989
_reflns_number_gt                5003
_reflns_number_total             5290
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00812_si_003.cif
_cod_data_source_block           Complex4
_cod_depositor_comments
'Adding full bibliography for 1520054--1520057.cif.'
_cod_database_code               1520055