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_4318310
_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            'C55 H118 Cl3 O7 P9 Si3 V3'
_chemical_formula_weight         1513.66
_chemical_name_systematic
;
?
;
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_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.072(6)
_cell_angle_beta                 82.975(6)
_cell_angle_gamma                74.774(5)
_cell_formula_units_Z            2
_cell_length_a                   10.6262(2)
_cell_length_b                   18.9290(4)
_cell_length_c                   20.7077(6)
_cell_measurement_reflns_used    15773
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.87
_cell_measurement_theta_min      2.24
_cell_volume                     3971.76(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.856
_diffrn_measured_fraction_theta_max 0.856
_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    0.0840
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
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_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.777
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1602
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     699
_refine_ls_number_reflns         16180
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_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.0756
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_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0629P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1187
_refine_ls_wR_factor_ref         0.1284
_reflns_number_gt                11150
_reflns_number_total             16180
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020041r_5.cif
_cod_data_source_block           shelxl/6
_cod_original_cell_volume        3971.77(16)
_cod_database_code               4318310