Homoleptic Isocyanidemetalates of 4d- and 5d-Transition Metals: [Nb(CNXyl)6]-, [Ta(CNXyl)6]-, and Derivatives Thereof1
Mikhail V. Barybin; William W. Brennessel; Benjamin E. Kucera; Mikhail E. Minyaev; Victor J. Sussman; Victor G. Young; John E. Ellis; Journal of the American Chemical Society 129 (2007) 1141–1150; doi:10.1021/ja065964q

data_4109046
_publ_contact_author_address
;Department of Chemistry
University of Minnesota
207 Pleasant St. SE
Minneapolis, MN 55455
USA
;
_publ_contact_author_email       ellis@chem.umn.edu
_publ_contact_author_name        'John E. Ellis'
_publ_contact_author_phone       001+612-625-6391
_publ_section_title
;
 Homoleptic Isocyanidemetalates of 4d- and 5d-Transition Metals:
 [Nb(CNXyl)6]-, [Ta(CNXyl)6]-, and Derivatives Thereof1
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1141
_journal_page_last               1150
_journal_paper_doi               10.1021/ja065964q
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C54 H54 Cs N6 Nb'
_chemical_formula_sum            'C54 H54 Cs N6 Nb'
_chemical_formula_weight         1012.85
_chemical_name_common
;
Cesium hexakis(2,6-dimethylphenylisocyanido)-niobium
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   23.504(3)
_cell_length_b                   23.504(3)
_cell_length_c                   7.7038(14)
_cell_measurement_reflns_used    3531
_cell_measurement_temperature    173(2)
_cell_volume                     3685.7(9)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens SMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            8245
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    1.016
_exptl_absorpt_correction_T_max  0.9323
_exptl_absorpt_correction_T_min  0.8226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       needle
_exptl_crystal_F_000             1548
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1464
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0847
_reflns_number_gt                1068
_reflns_number_total             1464
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja065964qsi20060823_114245_1.cif
_cod_data_source_block           00319
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4109046