Zirconium Complex of an [OSSO]-Type Diphenolate Ligand Bearing trans-1,2-Cyclooctanediylbis(thio) Core: Synthesis, Structure, and Isospecific 1-Hexene Polymerization
Akihiko Ishii; Tomoyuki Toda; Norio Nakata; Tsukasa Matsuo; Journal of the American Chemical Society 131 (2009) 13566–13567; doi:10.1021/ja903369q

data_4105056
_publ_section_title
;
 Zirconium Complex of an [OSSO]-Type Diphenolate Ligand Bearing
 trans-1,2-Cyclooctanediylbis(thio) Core: Synthesis, Structure, and
 Isospecific 1-Hexene Polymerization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13566
_journal_page_last               13567
_journal_paper_doi               10.1021/ja903369q
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C38 H60 O2 S2'
_chemical_formula_sum            'C38 H60 O2 S2'
_chemical_formula_weight         612.98
_chemical_name_common            C8H14[OSSO]H2
_chemical_name_systematic
; 
 C8H14[OSSO]H2 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 93.7270(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6866(5)
_cell_length_b                   10.8284(5)
_cell_length_c                   35.0668(18)
_cell_measurement_temperature    103(2)
_cell_volume                     3670.4(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0733
_diffrn_reflns_av_sigmaI/netI    0.0816
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            21828
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_T_max  0.9726
_exptl_absorpt_correction_T_min  0.9543
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_description       prism
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         6830
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0605
_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^)+(0.0638P)^2^+0.7338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1475
_reflns_number_gt                4727
_reflns_number_total             6830
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja903369q_si_002.cif
_cod_data_source_block           naka150
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4105056