Ethylene Polymerization Catalysis by Vanadium-Based Systems Bearing Sulfur-Bridged Calixarenes
Redshaw, Carl; Clowes, Lucy; Hughes, David L.; Elsegood, Mark R. J.; Yamato, Takehiko; Organometallics 30 (2011) 5620–; doi:10.1021/om200402u

data_4064904
_publ_section_title
;
 Ethylene Polymerization Catalysis by Vanadium-Based Systems Bearing
 Sulfur-Bridged Calixarenes
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5620
_journal_paper_doi               10.1021/om200402u
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety
'C40 H46 Cl2 O13 S4 V 1-, C24 H20 P 1+, 3(C H2 Cl2)'
_chemical_formula_sum            'C67 H72 Cl8 O13 P S4 V'
_chemical_formula_weight         1579.00
_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                85.5859(16)
_cell_angle_beta                 76.1046(16)
_cell_angle_gamma                74.8501(16)
_cell_formula_units_Z            2
_cell_length_a                   13.7043(16)
_cell_length_b                   16.4065(19)
_cell_length_c                   17.809(2)
_cell_measurement_reflns_used    10707
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.31
_cell_measurement_theta_min      2.28
_cell_volume                     3751.5(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31727
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1, Sheldrick, G.M., (2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.87
_exptl_crystal_size_mid          0.80
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.800
_refine_diff_density_min         -1.262
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1005
_refine_ls_number_reflns         15209
_refine_ls_number_restraints     575
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1016
_refine_ls_R_factor_gt           0.0677
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1180P)^2^+6.0824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1861
_refine_ls_wR_factor_ref         0.2188
_reflns_number_gt                10393
_reflns_number_total             15209
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om200402u_si_002.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4064904