Nitridotechnetium(V) Complexes with N-Heterocyclic Carbenes and Unexpected (OSiMe2OSiMe2O)2-Coligands
Braband, Henrik; Abram, Ulrich; Organometallics 24 (2005) 3362–; doi:10.1021/om050245q

data_4075887
_publ_section_title
;
 Nitridotechnetium(V) Complexes with N-Heterocyclic Carbenes and
 Unexpected (OSiMe2OSiMe2O)2-Coligands
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3362
_journal_paper_doi               10.1021/om050245q
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C36 H64 Cl2 N9 Tc1'
_chemical_formula_sum            'C36 H64 Cl2 N9 Tc'
_chemical_formula_weight         791.87
_chemical_name_systematic
;
Tetrakis{(1,3-diethyl-4,5-dimethyl)imidazolylyliden}nitridotechnetium(V) 
dichloride'
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.87(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.498(2)
_cell_length_b                   28.649(5)
_cell_length_c                   14.131(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.92
_cell_measurement_theta_min      9.36
_cell_volume                     4638.0(13)
_computing_cell_refinement       SET4
_computing_data_collection       CAD4
_computing_data_reduction        HELENA
_computing_molecular_graphics    ORTEP
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS 97'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       'omega scans'
_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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0618
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10557
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        5
_diffrn_standards_interval_count 400
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.458
_exptl_absorpt_correction_T_max  none
_exptl_absorpt_correction_T_min  none
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          .2
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .1
_refine_diff_density_max         1.093
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         9012
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_gt           0.0588
_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^)+(0.1398P)^2^+3.8280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1611
_refine_ls_wR_factor_ref         0.1984
_reflns_number_gt                6080
_reflns_number_total             9012
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050245qsi20050401_053408.cif
_cod_data_source_block           tcncarb4
_cod_original_cell_volume        4637.8(14)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C36 H64 Cl2 N9 Tc1'
_cod_database_code               4075887