Zirconium and hafnium complexes of the thio(bisphenolato) ligand: synthesis, structural characterization and testing as 1-hexene polymerization catalysts
Janas, Zofia; Godbole, Dorota; Nerkowski, Tomasz; Szczegot, Krzysztof; Dalton Transactions  (2009) 8846–8853; doi:10.1039/b907560g

data_7030602
_publ_section_title
;
 Zirconium and hafnium complexes of the thio(bisphenolato) ligand:
 synthesis, structural characterization and testing as 1-hexene
 polymerization catalysts
;
_journal_coden_ASTM              DTARAF
_journal_issue                   41
_journal_name_full               'Dalton Transactions'
_journal_page_first              8846
_journal_page_last               8853
_journal_paper_doi               10.1039/b907560g
_journal_year                    2009
_chemical_formula_moiety         'C56 H80 Al2 Cl6 O4 S2 Zr, 0.5(C6 H14)'
_chemical_formula_sum            'C59 H87 Al2 Cl6 O4 S2 Zr'
_chemical_formula_weight         1282.29
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                73.73(2)
_cell_angle_beta                 86.36(2)
_cell_angle_gamma                62.22(2)
_cell_formula_units_Z            2
_cell_length_a                   14.737(5)
_cell_length_b                   15.552(5)
_cell_length_c                   16.690(5)
_cell_measurement_reflns_used    7418
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     3238.6(19)
_computing_cell_refinement
'CrysAlis RED V1.171.3,Oxford Diffraction Ltd.,2006'
_computing_data_collection
'CrysAlis CCD V1.171.3,Oxford Diffraction Ltd.,2006'
_computing_data_reduction
' CrysAlis RED V1.171.3,Oxford Diffraction Ltd.,2006'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'SHELXTL V6.14, Bruker AXS 2003'
_computing_structure_refinement  'SHELXTL V6.14, Bruker AXS 2003'
_computing_structure_solution    'SHELXTL V6.14, Bruker AXS 2003'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Kuma KM-4 CCD kappa-axis diffractometer'
_diffrn_measurement_method       \w
_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  0.0538
_diffrn_reflns_av_sigmaI/netI    0.1212
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26815
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    0.551
_exptl_absorpt_correction_T_max  0.9124
_exptl_absorpt_correction_T_min  0.8230
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED V1.171.13, Oxford Diffraction Ltd.,
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
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_refine_diff_density_max         0.789
_refine_diff_density_min         -0.434
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         13944
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0507
_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^)+(0.0333P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0916
_reflns_number_gt                8625
_reflns_number_total             13944
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7002532
_cod_data_source_file            b907560g.txt
_cod_data_source_block           zj72
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        3239(2)
_cod_database_code               7030602