Vanadium-based imido-alkoxide pro-catalysts bearing bisphenolate ligands for ethylene and ε-caprolactone polymerisation
Arbaoui, Abdessamad; Redshaw, Carl; Homden, Damien M.; Wright, Joseph A.; Elsegood, Mark R. J.; Dalton Transactions  (2009) 8911–8922; doi:10.1039/b902402f

data_7002591
_publ_section_title
;
 Vanadium-based imido-alkoxide pro-catalysts bearing bisphenolate
 ligands for ethylene and \e-caprolactone polymerisation
;
_journal_issue                   41
_journal_name_full               'Dalton Transactions'
_journal_page_first              8911
_journal_page_last               8922
_journal_paper_doi               10.1039/b902402f
_journal_year                    2009
_chemical_formula_moiety         'C76 H106 Cl2 N2 O6 V2, C H2 Cl2'
_chemical_formula_structural     '[V(=NC6H4Cl)(diphenolate)(mu-O-Et)]2.CH2Cl2'
_chemical_formula_sum            'C77 H108 Cl4 N2 O6 V2'
_chemical_formula_weight         1401.33
_chemical_name_common            'Compound 10'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 99.969(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.0504(18)
_cell_length_b                   19.7366(19)
_cell_length_c                   20.978(2)
_cell_measurement_reflns_used    10491
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      24.9999
_cell_measurement_theta_min      3.0259
_cell_volume                     7768.4(13)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin <i>et al</i>, 1993)'
_computing_publication_material
;
SHELXL-97, PLATON (Spek, 2003), WinGX (Farrugia, 1999)
and enCIFer (Allen <i>et al.</i>, 2004)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1993)'
_diffrn_ambient_temperature      140(2)
_diffrn_detector_area_resol_mean 16.0050
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 3/CCD'
_diffrn_measurement_method       'Thin slice \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1336
_diffrn_reflns_av_sigmaI/netI    0.1390
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            83922
_diffrn_reflns_theta_full        25.17
_diffrn_reflns_theta_max         25.17
_diffrn_reflns_theta_min         3.03
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.427
_exptl_absorpt_correction_T_max  0.9284
_exptl_absorpt_correction_T_min  0.8764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSPACK; Oxford Diffraction, 2006)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2984
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.848
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     907
_refine_ls_number_reflns         13785
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      0.872
_refine_ls_R_factor_all          0.1267
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0243P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0792
_reflns_number_gt                7264
_reflns_number_total             13785
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b902402f.txt
_cod_data_source_block           10
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7002591