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_4325944
_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         'C108 H136 N2 O6 V2, 6(C2 H3 N)'
_chemical_formula_structural
'[{V(N-p-tol)(O-nPr)(OC6H2-tBu-CH2-C6H3-tBu)2}2].6(MeCN)'
_chemical_formula_sum            'C120 H154 N8 O6 V2'
_chemical_formula_weight         1906.39
_chemical_name_common            'Compound 2'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           1
_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                101.5039(12)
_cell_angle_beta                 103.0898(09)
_cell_angle_gamma                102.2226(11)
_cell_formula_units_Z            1
_cell_length_a                   12.0454(3)
_cell_length_b                   13.2444(2)
_cell_length_c                   19.3366(4)
_cell_measurement_reflns_used    126368
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2835.69(10)
_computing_cell_refinement       'EVAL-14 (Duisenberg, AJM, et al, 2003)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        'EVAL-14 (Duisenberg, AJM, et al, 2003)'
_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 '4096x4096 pixels/ 62x62 mm'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9970
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.220
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1284
_refine_ls_number_reflns         9970
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0685
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0273P)^2^+5.1150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1468
_refine_ls_wR_factor_ref         0.1541
_reflns_number_gt                9355
_reflns_number_total             9970
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic2010198_si_001_2.cif
_cod_data_source_block           twin5
_cod_database_code               4325944