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_4109049
_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 I N6 Ta'
_chemical_formula_sum            'C54 H54 I N6 Ta'
_chemical_formula_weight         1094.88
_chemical_name_common
;
Iodo-hexakis(2.6-dimethylphenylisocyanido)-tantalum
;
_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                 118.7690(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5129(6)
_cell_length_b                   40.725(2)
_cell_length_c                   11.7507(6)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    173(2)
_cell_volume                     4829.4(4)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker 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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            52781
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    2.957
_exptl_absorpt_correction_T_max  0.7978
_exptl_absorpt_correction_T_min  0.3995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_description       block
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.320
_refine_diff_density_min         -1.998
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         11019
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0230P)^2^+15.1543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0707
_reflns_number_gt                9907
_reflns_number_total             11019
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja065964qsi20060823_114245_4.cif
_cod_data_source_block           00250
_cod_database_code               4109049