Synthesis, structure and ethylene polymerisation behaviour of vanadium(iv and v) complexes bearing chelating aryloxides
Homden, Damien; Redshaw, Carl; Warford, Lee; Hughes, David L.; Wright, Joseph A.; Dale, Sophie H.; Elsegood, Mark R. J.; Dalton Transactions  (2009) 8900–8910; doi:10.1039/b901810g

data_7002595
_publ_section_title
;
 Synthesis, structure and ethylene polymerisation behaviour of
 vanadium(iv and v) complexes bearing chelating aryloxides
;
_journal_issue                   41
_journal_name_full               'Dalton Transactions'
_journal_page_first              8900
_journal_page_last               8910
_journal_paper_doi               10.1039/b901810g
_journal_year                    2009
_chemical_formula_moiety         'C56 H82 O8 S2 V2, 6(C2 H3 N)'
_chemical_formula_structural     '[V(=O)(S-diphenolate)(mu-OH)]2.6MeCN'
_chemical_formula_sum            'C68 H100 N6 O8 S2 V2'
_chemical_formula_weight         1295.54
_chemical_name_common            'Compound 3'
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4675(5)
_cell_length_b                   15.2783(5)
_cell_length_c                   29.5448(9)
_cell_measurement_reflns_used    17022
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.46
_cell_measurement_theta_min      2.28
_cell_volume                     7433.3(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'CAMERON (Watkins <i>et al.</i>, 1996)'
_computing_publication_material
;
Bruker SHELXTL (Sheldrick, 2008), PLATON (Spek, 2003), WinGX (Farrugia, 1999)
and enCIFer (Allen <i>et al.</i>, 2004)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            61637
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.360
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.10, Sheldrick, G.M., (2003)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         8500
_refine_ls_number_restraints     157
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+8.6736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1309
_reflns_number_gt                6221
_reflns_number_total             8500
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b901810g.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7002595