Vanadium-Based Pro-Catalysts Bearing Depleted 1,3-Calix[4]arenes for Ethylene or ε-Caprolactone Polymerization
Lucy Clowes; Carl Redshaw; David L. Hughes; Inorganic Chemistry 50 (2011) 7838–7845; doi:10.1021/ic2010198

data_4325945
_publ_section_title
;
 Vanadium-Based Pro-Catalysts Bearing Depleted 1,3-Calix[4]arenes for
 Ethylene or \e-Caprolactone Polymerization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7838
_journal_page_last               7845
_journal_paper_doi               10.1021/ic2010198
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         '3(C110 H140 N2 O6 V2), ca 11(C2 H3 N)'
_chemical_formula_structural
'3[{V(N-p-tol)(O-tBu)(OC6H2-tBu-CH2-C6H3-tBu)2}2].ca 11(MeCN)'
_chemical_formula_sum            'C352 H453 N17 O18 V6'
_chemical_formula_weight         5515.95
_chemical_name_common            'Compound 3'
_chemical_name_systematic
;
 ?
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.5872(14)
_cell_angle_beta                 83.260(2)
_cell_angle_gamma                81.467(2)
_cell_formula_units_Z            2
_cell_length_a                   12.1955(8)
_cell_length_b                   27.1953(19)
_cell_length_c                   50.486(4)
_cell_measurement_reflns_used    93700
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.91
_cell_volume                     16164(2)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_molecular_graphics    'ORTEP (Johnson, 1971 and Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean '4096 x 4096 pixels/62 x 62 mm'
_diffrn_measured_fraction_theta_full 0.857
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_device_type
'Bruker-Nonius APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  '10 cm confocal mirrors'
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1313
_diffrn_reflns_av_sigmaI/netI    0.2205
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            74299
_diffrn_reflns_theta_full        20.00
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_description       lath
_exptl_crystal_F_000             5932
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1789
_refine_ls_number_reflns         25893
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.2997
_refine_ls_R_factor_gt           0.1683
_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^)+(0.0209P)^2^+384.3127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2889
_refine_ls_wR_factor_ref         0.3417
_reflns_number_gt                12761
_reflns_number_total             25893
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic2010198_si_001_3.cif
_cod_data_source_block           2010src1034
_cod_original_cell_volume        16164.4(19)
_cod_database_code               4325945