Paramagnetic Vanadium Silyl Complexes: Synthesis, Structure, and Reactivity
Shinohara, Akihiro; McBee, Jennifer; Waterman, Rory; Tilley, T. Don; Organometallics 27 (2008) 5717–; doi:10.1021/om800712k

data_4072264
_publ_section_title
;
 Paramagnetic Vanadium Silyl Complexes: Synthesis, Structure, and
 Reactivity
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5717
_journal_paper_doi               10.1021/om800712k
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C23 H31 Cl2 P2 Si V, C6 H6'
_chemical_formula_sum            'C29 H37 Cl2 P2 Si V'
_chemical_formula_weight         597.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.4240(13)
_cell_length_b                   9.4930(7)
_cell_length_c                   17.8481(14)
_cell_measurement_reflns_used    2093
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.82
_cell_measurement_theta_min      2.43
_cell_volume                     2952.2(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0775
_diffrn_reflns_av_sigmaI/netI    0.1689
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16012
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  .91
_exptl_absorpt_correction_T_min  .84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs, 2004'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.632
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5410
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.632
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0082P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0543
_refine_ls_wR_factor_ref         0.0564
_reflns_number_gt                2943
_reflns_number_total             5410
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800712k_si_003.cif
_cod_data_source_block           aki4s
_cod_original_sg_symbol_H-M      Pna2(1)
_cod_database_code               4072264