Synthesis of Alkyl and Alkylidene Complexes of Tungsten Bearing Imido and Redox-Active α-Diimine oro-Iminoquinone Ligands and Their Application as Catalysts for Ring-Opening Metathesis Polymerization of Norbornene
Tanahashi, Hiromasa; Tsurugi, Hayato; Mashima, Kazushi; Organometallics 34 (2015) 731–; doi:10.1021/om501010n

data_4085503
_publ_section_title
;
 Synthesis of Alkyl and Alkylidene Complexes of Tungsten Bearing Imido and
 Redox-Active \a-Diimine oro-Iminoquinone Ligands and Their Application as
 Catalysts for Ring-Opening Metathesis Polymerization of Norbornene
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              731
_journal_paper_doi               10.1021/om501010n
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C53 H70 N3 P W'
_chemical_formula_sum            'C53 H70 N3 P W'
_chemical_formula_weight         963.94
_chemical_name_common            6
_chemical_name_systematic
; 
 ? 
;
_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                 93.881(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.372(4)
_cell_length_b                   12.360(4)
_cell_length_c                   35.044(11)
_cell_measurement_reflns_used    10115
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.22
_cell_volume                     5347(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0777
_diffrn_reflns_av_sigmaI/netI    0.0794
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            49948
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         3.22
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.223
_exptl_absorpt_correction_T_max  0.8422
_exptl_absorpt_correction_T_min  0.6903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         4.403
_refine_diff_density_min         -2.557
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         12241
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.1049
_refine_ls_R_factor_gt           0.0877
_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^)+(0.0910P)^2^+26.2590P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2145
_refine_ls_wR_factor_ref         0.2304
_reflns_number_gt                9995
_reflns_number_total             12241
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501010n_si_001.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 4085499--4085505.cif.'
_cod_database_code               4085503