Synthesis, Structure, and 1-Hexene Polymerization Catalytic Ability of Group 5 Metal Complexes Incorporating an [OSSO]-Type Ligand
Toda, Tomoyuki; Nakata, Norio; Matsuo, Tsukasa; Ishii, Akihiko; ACS Catalysis 3 (2013) 1764–; doi:10.1021/cs4003996

data_4508111
_publ_section_title
;
 Synthesis, Structure, and 1-Hexene Polymerization Catalytic Ability of
 Group 5 Metal Complexes Incorporating an [OSSO]-Type Ligand
;
_journal_issue                   8
_journal_name_full               'ACS Catalysis'
_journal_page_first              1764
_journal_paper_doi               10.1021/cs4003996
_journal_volume                  3
_journal_year                    2013
_chemical_formula_moiety         'C38 H58 Cl3 Nb O2 S2, 0.5(C12), 2(C6 H6)'
_chemical_formula_sum            'C56 H70 Cl3 Nb O2 S2'
_chemical_formula_weight         1038.50
_chemical_name_common            C8H14[OSSO]NbCl3
_chemical_name_systematic
; 
 C8H14[OSSO]NbCl3 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 103.391(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.747(5)
_cell_length_b                   15.722(4)
_cell_length_c                   19.957(6)
_cell_measurement_temperature    100(2)
_cell_volume                     5417(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'ORTEP-3 for Windows'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SIR-2004
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku AFC-8 with Saturn70 CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_sigmaI/netI    0.0552
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37950
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    0.486
_exptl_absorpt_correction_T_max  0.9714
_exptl_absorpt_correction_T_min  0.9091
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         10048
_refine_ls_number_restraints     217
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+5.7992P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1659
_reflns_number_gt                7801
_reflns_number_total             10048
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs4003996_si_003.cif
_cod_data_source_block           riken16
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4508111