Amine influence in vanadium-based ethylene polymerisation pro-catalysts bearing bis(phenolate) ligands with ‘pendant’ arms
Lorber, Christian; Despagnet-Ayoub, Emmanuelle; Vendier, Laure; Arbaoui, Abdessamad; Redshaw, Carl; Catalysis Science & Technology 1 (2011) 489–; doi:10.1039/c1cy00089f

data_1556281
_publ_section_title
;
 Amine influence in vanadium-based ethylene polymerisation pro-catalysts
 bearing bis(phenolate) ligands with &#x2018;pendant&#x2019; arms
;
_journal_issue                   3
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              489
_journal_paper_doi               10.1039/c1cy00089f
_journal_volume                  1
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C24 H34 N1 O4 V1'
_chemical_formula_sum            'C24 H34 N O4 V'
_chemical_formula_weight         451.46
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 94.873(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4832(12)
_cell_length_b                   11.5025(16)
_cell_length_c                   24.140(3)
_cell_measurement_reflns_used    2431
_cell_measurement_temperature    180
_cell_measurement_theta_max      27.999
_cell_measurement_theta_min      2.6324
_cell_measurement_wavelength     0.71073
_cell_volume                     2347.0(6)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur'
_diffrn_measurement_method       \w-\f
_diffrn_orient_matrix_UB_11      -0.0078759959
_diffrn_orient_matrix_UB_12      -0.0005810484
_diffrn_orient_matrix_UB_13      0.0291892969
_diffrn_orient_matrix_UB_21      -0.0833417934
_diffrn_orient_matrix_UB_22      0.007749268
_diffrn_orient_matrix_UB_23      -0.0052735623
_diffrn_orient_matrix_UB_31      -0.0104704705
_diffrn_orient_matrix_UB_32      -0.0615616867
_diffrn_orient_matrix_UB_33      -0.0009645225
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1848
_diffrn_reflns_av_unetI/netI     0.192
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            16030
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.83
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.451
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.27 (release 29-05-2008 CrysAlis171 .NET)
(compiled May 29 2008,13:12:44)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         4289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.1833
_refine_ls_R_factor_gt           0.0681
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1377
_reflns_number_gt                1908
_reflns_number_total             4289
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c1cy00089f.txt
_cod_data_source_block           3
_cod_database_code               1556281