Role of Axial Base Coordination in Isonitrile Binding and Chalcogen Atom Transfer to Vanadium(III) Complexes.
Majumdar, Subhojit; Stauber, Julia M.; Palluccio, Taryn D.; Cai, Xiaochen; Velian, Alexandra; Rybak-Akimova, Elena V; Temprado, Manuel; Captain, Burjor; Cummins, Christopher C.; Hoff, Carl D.; Inorganic chemistry  (2014) 141003140335004–; doi:10.1021/ic5017005

data_4341204
_publ_section_title
;
 Role of Axial Base Coordination in Isonitrile Binding and Chalcogen Atom
 Transfer to Vanadium(III) Complexes.
;
_journal_name_full               'Inorganic chemistry'
_journal_page_first              141003140335004
_journal_paper_doi               10.1021/ic5017005
_journal_year                    2014
_chemical_formula_sum            'C15 H39 N4 O Si3 V'
_chemical_formula_weight         426.71
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-2012
_cell_angle_alpha                66.3410(10)
_cell_angle_beta                 89.977(2)
_cell_angle_gamma                79.480(2)
_cell_formula_units_Z            4
_cell_length_a                   9.6971(6)
_cell_length_b                   16.2957(10)
_cell_length_c                   16.5852(10)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.31
_cell_volume                     2352.4(3)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.943
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17550
_diffrn_reflns_point_group_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.559
_diffrn_reflns_theta_min         1.345
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_T_max  0.746070
_exptl_absorpt_correction_T_min  0.566916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         17550
_refine_ls_number_restraints     750
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+1.9724P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.0969
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16078
_reflns_number_total             17550
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5017005_si_003.cif
_cod_data_source_block           x13085_t5
_cod_database_code               4341204
_shelx_estimated_absorpt_t_min   0.892
_shelx_estimated_absorpt_t_max   0.944
_shelxl_version_number           2012-9
_shelx_res_checksum              27852
_shelx_hkl_checksum              42742