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_7002597
_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         'C63 H96 O8 V2'
_chemical_formula_structural     '[{V(=O)(diphenolate)}2(mu-OH)(mu-OPr)]'
_chemical_formula_sum            'C63 H96 O8 V2'
_chemical_formula_weight         1083.28
_chemical_name_common            'Compound 5'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   'geom except OH coords freely refined'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 108.4160(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.2469(7)
_cell_length_b                   24.3672(11)
_cell_length_c                   18.2970(8)
_cell_measurement_reflns_used    13303
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.10
_cell_measurement_theta_min      2.26
_cell_volume                     6449.7(5)
_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 1.000
_diffrn_measured_fraction_theta_max 0.905
_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  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28550
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.09
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.338
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03, Sheldrick, G.M., (2001)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         7835
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+5.5517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1119
_reflns_number_gt                6188
_reflns_number_total             7835
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b901810g.txt
_cod_data_source_block           5
_cod_original_cell_volume        6449.6(5)
_cod_original_sg_symbol_H-M      I2/a
_cod_database_code               7002597