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_4325946
_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         'C100 H136 O14 V4,2(C2H3N)'
_chemical_formula_structural
'[{V2O2(m3-O)(m-OnPr)(OnPr)(calix,C44H54O2)}2].2(MeCN)'
_chemical_formula_sum            'C104 H142 N2 O14 V4'
_chemical_formula_weight         1847.96
_chemical_name_common            'Compound 4'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           'SHELXL-97 and CrysAlisPro RED'
_cell_angle_alpha                90.00
_cell_angle_beta                 106.105(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.3632(7)
_cell_length_b                   21.7638(10)
_cell_length_c                   19.9295(12)
_cell_measurement_reflns_used    5865
_cell_measurement_temperature    140(1)
_cell_measurement_theta_max      25.0000
_cell_measurement_theta_min      3.4211
_cell_volume                     5152.0(5)
_computing_cell_refinement
;
 CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.33.55 
;
_computing_data_collection
;
 CrysAlisPro CCD, Oxford Diffraction Ltd., Version 1.171.33.55 
;
_computing_data_reduction
;
 CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.33.55
;
_computing_molecular_graphics    'ORTEP (Johnson, 1976 and Farrugia, 1997)'
_computing_publication_material
'SHELXL-97 (Sheldrick, 2008) and WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      140(1)
_diffrn_detector_area_resol_mean 16.0050
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 3/Sapphire3 CCD'
_diffrn_measurement_method       'Thin slice \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1796
_diffrn_reflns_av_sigmaI/netI    0.1663
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            58567
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         3.43
_exptl_absorpt_coefficient_mu    0.411
_exptl_absorpt_correction_T_max  1.024
_exptl_absorpt_correction_T_min  0.966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.33.55 
 empirical absorption correction using spherical harmonics,
  implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'deep red'
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_description       plate
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         6711
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.921
_refine_ls_R_factor_all          0.1410
_refine_ls_R_factor_gt           0.0663
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0699P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1387
_refine_ls_wR_factor_ref         0.1560
_reflns_number_gt                3440
_reflns_number_total             6711
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic2010198_si_001_4.cif
_cod_data_source_block           lucyc13a
_cod_original_formula_sum        'C104 H142 O14 N2 V4'
_cod_database_code               4325946