Neutral Methyl and Cationic Aluminum Complexes Supported by atrans-1,2-Cyclooctanediyl-Bridged [OSSO]-Type Bis(phenolato) Ligand: Synthesis, Structures, and Use in Catalysis for Propylene Oxide Polymerization
Nakata, Norio; Saito, Yusuke; Ishii, Akihiko; Organometallics 33 (2014) 1840–; doi:10.1021/om5001698

data_4082796
_publ_section_title
;
 Neutral Methyl and Cationic Aluminum Complexes Supported by
 atrans-1,2-Cyclooctanediyl-Bridged [OSSO]-Type Bis(phenolato) Ligand:
 Synthesis, Structures, and Use in Catalysis for Propylene Oxide
 Polymerization
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1840
_journal_paper_doi               10.1021/om5001698
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety
'C76 H116 Al2 O4 S4, 2(C19 H3 B F15), 3.5(C6 H6)'
_chemical_formula_sum            'C135 H143 Al2 B2 F30 O4 S4'
_chemical_formula_weight         2603.31
_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                79.5170(10)
_cell_angle_beta                 82.1260(10)
_cell_angle_gamma                82.7930(10)
_cell_formula_units_Z            2
_cell_length_a                   16.8797(15)
_cell_length_b                   17.8986(16)
_cell_length_c                   21.649(2)
_cell_measurement_temperature    90(2)
_cell_volume                     6336.8(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0858
_diffrn_reflns_av_sigmaI/netI    0.0698
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31526
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    0.187
_exptl_absorpt_correction_T_max  0.9707
_exptl_absorpt_correction_T_min  0.9548
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2710
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1620
_refine_ls_number_reflns         23067
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0715P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1254
_reflns_number_gt                18141
_reflns_number_total             23067
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5001698_si_002.cif
_cod_data_source_block           compound5+
_cod_depositor_comments
;Adding full bibliography for 4082796.cif.

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_cell_volume        6336.9(10)
_cod_database_code               4082796