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_4318307
_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_moiety         'C15 H33 N Nb O3 P3 Si '
_chemical_formula_sum            'C15 H33 N Nb O3 P3 Si'
_chemical_formula_weight         489.34
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_audit_creation_date             1997-11-25
_audit_creation_method           'by teXsan v1.8'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5158(10)
_cell_length_b                   13.6408(8)
_cell_length_c                   10.426(2)
_cell_measurement_reflns_used    16152
_cell_measurement_temperature    180.2
_cell_measurement_theta_max      30.06
_cell_measurement_theta_min      1.93
_cell_volume                     2348.9(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1993)
;
_diffrn_ambient_temperature      180.2
_diffrn_measurement_device_type  'Quantum CCD'
_diffrn_measurement_method       'area detector'
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.02794
_diffrn_reflns_av_sigmaI/netI    0.0714
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            16225
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         2.31
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.780
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.921
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1016.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.94
_refine_diff_density_min         -1.57
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.997
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         3483
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.053
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0844P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1401
_refine_ls_wR_factor_ref         0.1488
_reflns_number_gt                2322
_reflns_number_total             3483
_reflns_threshold_expression     I>2.00\s(I)
_cod_data_source_file            ic020041r_2.cif
_cod_data_source_block           pl173/JCNB1/3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2348.8(6)
_cod_original_sg_symbol_H-M      'P n m a '
_cod_original_formula_sum        'C15 H33 N Nb O3 P3 Si '
_cod_database_code               4318307