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_4075888
_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         'C22 H44 N5 O3 Si2 Tc'
_chemical_formula_sum            'C22 H44 N5 O3 Si2 Tc'
_chemical_formula_weight         580.80
_chemical_name_systematic
;
Bis{(1,3-Diethyl-4,5-dimethyl)imidazolylyliden}-
(1,1,3,3-tetramethyldisiloxane-1,3-diolato)nitridotechnetium(V)

;
_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                 95.44(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.057(2)
_cell_length_b                   18.112(3)
_cell_length_c                   15.597(3)
_cell_measurement_reflns_used    984
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.421
_cell_measurement_theta_min      3.359
_cell_volume                     2828.2(9)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        SAINT
_computing_molecular_graphics    ORTEP
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Smart'
_diffrn_measurement_method       'phi and 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  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34332
_diffrn_reflns_theta_full        30.55
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '10 sec / frame'
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  none
_exptl_absorpt_correction_T_min  none
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          .58
_exptl_crystal_size_mid          .43
_exptl_crystal_size_min          .43
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         8631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+4.2741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0842
_reflns_number_gt                7632
_reflns_number_total             8631
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050245qsi20050401_053408.cif
_cod_data_source_block           tcnc2si
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4075888