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_1520054
_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         'C26 H33 Cl4 N5 Nb2'
_chemical_formula_sum            'C26 H33 Cl4 N5 Nb2'
_chemical_formula_weight         743.19
_chemical_name_common            complex3
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.548(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.913(2)
_cell_length_b                   13.362(2)
_cell_length_c                   15.947(3)
_cell_measurement_reflns_used    5530
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.34
_cell_measurement_theta_min      3.05
_cell_volume                     3374.9(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1102
_diffrn_reflns_av_sigmaI/netI    0.1034
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31527
_diffrn_reflns_theta_full        27.28
_diffrn_reflns_theta_max         27.28
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    1.018
_exptl_absorpt_correction_T_max  0.9604
_exptl_absorpt_correction_T_min  0.8623
_exptl_crystal_colour            red-Purple
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.011
_refine_diff_density_min         -1.064
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.274
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         7546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.274
_refine_ls_R_factor_all          0.1479
_refine_ls_R_factor_gt           0.1186
_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^)+(0.0672P)^2^+19.7646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2268
_refine_ls_wR_factor_ref         0.2474
_reflns_number_gt                5933
_reflns_number_total             7546
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00812_si_003.cif
_cod_data_source_block           complex3
_cod_depositor_comments
'Adding full bibliography for 1520054--1520057.cif.'
_cod_original_cell_volume        3374.8(10)
_cod_database_code               1520054