Synthesis and Characterization of Paramagnetic Tungsten Imido Complexes Bearing α-Diimine Ligands.
Tanahashi, Hiromasa; Ikeda, Hideaki; Tsurugi, Hayato; Mashima, Kazushi; Inorganic chemistry 55 (2016) 1446–1452; doi:10.1021/acs.inorgchem.5b02145

data_4346796
_publ_section_title
;
 Synthesis and Characterization of Paramagnetic Tungsten Imido Complexes
 Bearing \a-Diimine Ligands.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1446
_journal_page_last               1452
_journal_paper_doi               10.1021/acs.inorgchem.5b02145
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C48 H57 Cl3 N3 W, C6 H6, 1.5(C6 H14)'
_chemical_formula_sum            'C63 H84 Cl3 N3 W'
_chemical_formula_weight         1173.53
_chemical_name_common            6
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                89.723(9)
_cell_angle_beta                 73.401(9)
_cell_angle_gamma                73.312(8)
_cell_formula_units_Z            2
_cell_length_a                   11.842
_cell_length_b                   12.9906(5)
_cell_length_c                   20.7172(8)
_cell_measurement_reflns_used    7122
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.07
_cell_volume                     2915.2(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0612
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28202
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.09
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.159
_exptl_absorpt_correction_T_max  0.5733
_exptl_absorpt_correction_T_min  0.4501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.29
_refine_diff_density_max         3.157
_refine_diff_density_min         -1.927
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         12985
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0288P)^2^+4.9590P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0984
_reflns_number_gt                11272
_reflns_number_total             12985
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02145_si_002.cif
_cod_data_source_block           complex6
_cod_original_cell_volume        2915.26(16)
_cod_database_code               4346796