Group 5 hydride and borohydride complexes supported by cyclopentadienyl-imido ligand sets.
McLeod, Nicolas A.; Kuzmina, Lyudmila G.; Churakov, Andrei V.; Mountford, Philip; Nikonov, Georgii I.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 188–195; doi:10.1039/c3dt52489b

data_7029240
_publ_section_title
;
 Group 5 hydride and borohydride complexes supported by
 cyclopentadienyl-imido ligand sets.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              188
_journal_page_last               195
_journal_paper_doi               10.1039/c3dt52489b
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C34 H52 B2 N2 Nb2'
_chemical_formula_sum            'C34 H52 B2 N2 Nb2'
_chemical_formula_weight         696.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.568(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6798(2)
_cell_length_b                   20.3557(5)
_cell_length_c                   15.7752(3)
_cell_measurement_reflns_used    8094
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.39
_cell_measurement_theta_min      2.38
_cell_volume                     3406.94(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22730
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_T_max  0.63503
_exptl_absorpt_correction_T_min  0.51133
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       red
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.950
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         7437
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0283P)^2^+4.7322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0865
_reflns_number_gt                6366
_reflns_number_total             7437
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3dt52489b.txt
_cod_data_source_block           xx
_cod_original_cell_volume        3406.9(1)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7029240