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_7002598
_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         'C60 H90 O8 V2, 4(C2 H3 N)'
_chemical_formula_structural     '[V(=O)(diphenolate)(mu-OH)]2.4MeCN'
_chemical_formula_sum            'C68 H102 N4 O8 V2'
_chemical_formula_weight         1205.42
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   'geom except H1 coords freely refined'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                71.2558(10)
_cell_angle_beta                 74.5933(10)
_cell_angle_gamma                68.2679(10)
_cell_formula_units_Z            1
_cell_length_a                   10.5991(7)
_cell_length_b                   12.9675(8)
_cell_length_c                   14.7112(9)
_cell_measurement_reflns_used    9175
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.76
_cell_measurement_theta_min      2.27
_cell_volume                     1753.73(19)
_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 0.991
_diffrn_measured_fraction_theta_max 0.864
_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  0.0169
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15504
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.318
_exptl_absorpt_correction_T_max  0.870
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, G.M., (2003)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.98
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         8073
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0503P)^2^+0.7320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1038
_reflns_number_gt                6816
_reflns_number_total             8073
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b901810g.txt
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7002598