Group 4 complexes of a new [OSSO]-type dianionic ligand. Coordination chemistry and preliminary polymerization catalysis studies.
Cohen, Ad; Yeori, Adi; Goldberg, Israel; Kol, Moshe; Inorganic chemistry 46 (2007) 8114–8116; doi:10.1021/ic701370t

data_4339447
_publ_section_title
;
 Group 4 complexes of a new [OSSO]-type dianionic ligand. Coordination
 chemistry and preliminary polymerization catalysis studies.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8114
_journal_page_last               8116
_journal_paper_doi               10.1021/ic701370t
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C40 H66 O4 S2 Zr, C2.5 H5.5'
_chemical_formula_sum            'C42.5 H71.5 O4 S2 Zr'
_chemical_formula_weight         801.84
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 93.0593(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0206(2)
_cell_length_b                   17.7528(2)
_cell_length_c                   19.5067(4)
_cell_measurement_reflns_used    10275
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      1.41
_cell_volume                     4502.59(13)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B.V.'
_computing_data_reduction        'Denzo & Scalepack'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 12.8
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. \f & \w 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  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40493
_diffrn_reflns_theta_full        28.06
_diffrn_reflns_theta_max         28.06
_diffrn_reflns_theta_min         2.09
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.373
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1722
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         10709
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0717P)^2^+0.7764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1314
_reflns_number_gt                7745
_reflns_number_total             10709
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701370t-file003.cif
_cod_data_source_block           mk176
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C42.50 H71.50 O4 S2 Zr'
_cod_database_code               4339447