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_4325943
_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         'C94 H118 O8 V2, ca 4(C2 H3 N)'
_chemical_formula_structural
'[{V O (OiPr) (calix, C44H54O2)}2].ca 4(MeCN)'
_chemical_formula_sum            'C102 H130 N4 O8 V2'
_chemical_formula_weight         1641.98
_chemical_name_common            'Compound 1'
_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 and CrysAlisPro RED'
_cell_angle_alpha                86.074(3)
_cell_angle_beta                 77.914(3)
_cell_angle_gamma                80.074(3)
_cell_formula_units_Z            2
_cell_length_a                   12.5484(4)
_cell_length_b                   19.6001(6)
_cell_length_c                   20.2006(9)
_cell_measurement_reflns_used    7590
_cell_measurement_temperature    140(1)
_cell_measurement_theta_max      25.9998
_cell_measurement_theta_min      3.3987
_cell_volume                     4782.8(3)
_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  0.0996
_diffrn_reflns_av_sigmaI/netI    0.1951
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50213
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         3.41
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_T_max  1.034
_exptl_absorpt_correction_T_min  0.976
_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            red
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_description       plate
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.755
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1064
_refine_ls_number_reflns         12464
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.755
_refine_ls_R_factor_all          0.1215
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.181
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0875
_reflns_number_gt                5860
_reflns_number_total             12464
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic2010198_si_001_1.cif
_cod_data_source_block           lucyc13
_cod_database_code               4325943