Synthesis, Characterization, and Solution Redox Properties of (trimpsi)M(CO)2(NO) Complexes [M = V, Nb, Ta; trimpsi = tBuSi(CH2PMe2)3]
Trevor W. Hayton; P. James Daff; Peter Legzdins; Steven J. Rettig; Brian O. Patrick; Inorganic Chemistry 41 (2002) 4114–4126; doi:10.1021/ic020041r

data_4318309
_publ_contact_author_address
;
University of British Columbia
Department of Chemistry
2036 Main Mall
Vancouver, BC V6T 1Z1
Canada
;
_publ_contact_author_email       ' legzdins@chem.ubc.ca '
_publ_contact_author_fax         ' 604-822-2847 '
_publ_contact_author_name        ' Prof. Peter Legzdins'
_publ_contact_author_phone       ' 604-822-2987 '
_publ_section_title
;
 Synthesis, Characterization, and Solution Redox Properties of
 (trimpsi)M(CO)2(NO) Complexes [M = V, Nb, Ta; trimpsi = tBuSi(CH2PMe2)3]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4114
_journal_page_last               4126
_journal_paper_doi               10.1021/ic020041r
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C18 H37 I O3.5 P3 Si Ta'
_chemical_formula_weight         738.33
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 108.8490(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   37.2045(6)
_cell_length_b                   9.7244(3)
_cell_length_c                   17.9893(4)
_cell_measurement_reflns_used    17433
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.59
_cell_measurement_theta_min      3.09
_cell_volume                     6159.4(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.817
_diffrn_measured_fraction_theta_max 0.817
_diffrn_measurement_device_type  'Rigaku/ADSC CCD'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7073
_diffrn_reflns_theta_full        29.59
_diffrn_reflns_theta_max         29.59
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    4.782
_exptl_absorpt_correction_T_max  0.7009
_exptl_absorpt_correction_T_min  0.2854
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.608
_refine_diff_density_min         -1.674
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.888
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         7073
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      0.888
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          1.667
_refine_ls_shift/su_mean         0.067
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+15.9455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0768
_reflns_number_gt                6066
_reflns_number_total             7073
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020041r_4.cif
_cod_data_source_block           pl221/2.1/2THF
_cod_original_formula_sum        'C18 H37 I O3.50 P3 Si Ta'
_cod_database_code               4318309