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_4085499
_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         'C38 H53 Cl3 N3 W, C16 H36 N'
_chemical_formula_sum            'C54 H89 Cl3 N4 W'
_chemical_formula_weight         1084.49
_chemical_name_common            2
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_symmetry_cell_setting           monoclinic
_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                 94.813(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.476(12)
_cell_length_b                   11.704(6)
_cell_length_c                   22.069(12)
_cell_measurement_reflns_used    6594
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.08
_cell_volume                     5528(5)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_publication_material  'CrystalStructure 4.1'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1407
_diffrn_reflns_av_sigmaI/netI    0.1272
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            41999
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.08
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.271
_exptl_absorpt_correction_T_max  0.8572
_exptl_absorpt_correction_T_min  0.5123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2264
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         6.889
_refine_diff_density_min         -2.166
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         9698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1584
_refine_ls_R_factor_gt           0.1067
_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^)+(0.1801P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2629
_refine_ls_wR_factor_ref         0.3146
_reflns_number_gt                5858
_reflns_number_total             9698
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501010n_si_001.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 4085499--4085505.cif.'
_cod_database_code               4085499