Volatile Imido−Hydrazido Compounds of the Refractory Metals Niobium, Tantalum, Molybdenum, and Tungsten
Gaess, Daniel; Harms, Klaus; Pokoj, Michael; Stolz, Wolfgang; Sundermeyer, Jörg; Inorganic Chemistry 46 (2007) 6688–6701; doi:10.1021/ic062435e

data_4333212
_publ_section_title
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 Volatile Imido&#x2212;Hydrazido Compounds of the Refractory Metals
 Niobium, Tantalum, Molybdenum, and Tungsten
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_journal_issue                   16
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6688
_journal_page_last               6701
_journal_paper_doi               10.1021/ic062435e
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C21 H46 N5 Si2 Ta'
_chemical_formula_sum            'C21 H46 N5 Si2 Ta'
_chemical_formula_weight         605.76
_chemical_name_systematic
;

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_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                 94.528(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.5882(12)
_cell_length_b                   10.3497(4)
_cell_length_c                   15.9474(10)
_cell_measurement_reflns_used    38240
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.3
_cell_measurement_theta_min      1.3
_cell_volume                     2893.9(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_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  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            39968
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    3.896
_exptl_absorpt_correction_T_max  0.7186
_exptl_absorpt_correction_T_min  0.364
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.00066(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         5623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0222
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0521
_refine_ls_wR_factor_ref         0.0534
_reflns_number_gt                4755
_reflns_number_total             5623
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062435esup1.cif
_cod_data_source_block           compound_5a
_cod_database_code               4333212