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_4318306
_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 O3 P3 Si Ta '
_chemical_formula_sum            'C15 H33 N O3 P3 Si Ta'
_chemical_formula_weight         577.39
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             2002-01-14
_audit_creation_method           'by teXsan v1.8'
_cell_angle_alpha                90
_cell_angle_beta                 101.5387(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7532(14)
_cell_length_b                   17.5506(15)
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_cell_measurement_reflns_used    17441
_cell_measurement_temperature    180.2
_cell_measurement_theta_max      30.0
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_cell_volume                     2386.0(4)
_computing_cell_refinement       'd*TREK (MSC, 1996-1998)'
_computing_data_collection       'd*TREK (MSC, 1996-1998)'
_computing_data_reduction        'd*TREK (MSC, 1996-1998)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
DIRDIF92 PATTY (Beurskens, 1992)
;
_diffrn_ambient_temperature      180.2
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_diffrn_measurement_device_type  'Rigaku/ADSC CCD'
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_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
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_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
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_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  0.03700
_diffrn_reflns_av_sigmaI/netI    0.0657
_diffrn_reflns_limit_h_max       12
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_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22182
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         30.66
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.863
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_exptl_absorpt_correction_T_min  0.357
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
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_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
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_refine_diff_density_min         -3.09
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.964
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         6052
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0714
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_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0767P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1218
_reflns_number_gt                4227
_reflns_number_total             6052
_reflns_threshold_expression     I>2.00\s(I)
_cod_data_source_file            ic020041r_1.cif
_cod_data_source_block           pl169/JDTA1/4
_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        2386.0(3)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C15 H33 N O3 P3 Si Ta '
_cod_database_code               4318306