5d Early-Transition-Metal Corroles: a Trioxo-Bridged Binuclear Tungsten(VI) Derivative
Izana Nigel-Etinger; Israel Goldberg; Zeev Gross; Inorganic Chemistry 51 (2012) 1983–1985; doi:10.1021/ic202325h

data_4328376
_publ_section_title
;
 5d Early-Transition-Metal Corroles: a Trioxo-Bridged Binuclear
 Tungsten(VI) Derivative
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1983
_journal_page_last               1985
_journal_paper_doi               10.1021/ic202325h
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C74 H16 F30 N8 O3 W2'
_chemical_formula_sum            'C74 H16 F30 N8 O3 W2'
_chemical_formula_weight         2002.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                95.614(5)
_cell_angle_beta                 97.520(5)
_cell_angle_gamma                108.921(5)
_cell_formula_units_Z            2
_cell_length_a                   12.2271(7)
_cell_length_b                   16.5676(12)
_cell_length_c                   18.7326(18)
_cell_measurement_reflns_used    8544
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.41
_cell_volume                     3518.8(5)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B.V.'
_computing_data_reduction        'Denzo & Scalepack'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 12.8
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '0.3 deg. \w 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  0.0605
_diffrn_reflns_av_sigmaI/netI    0.0688
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26625
_diffrn_reflns_theta_full        25.13
_diffrn_reflns_theta_max         25.13
_diffrn_reflns_theta_min         2.40
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.402
_exptl_absorpt_correction_T_max  0.6293
_exptl_absorpt_correction_T_min  0.3822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.890
_exptl_crystal_description       prism
_exptl_crystal_F_000             1916
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
;
_refine_diff_density_max         2.596
_refine_diff_density_min         -1.378
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1054
_refine_ls_number_reflns         12319
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0653P)^2^+2.6735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1488
_reflns_number_gt                8679
_reflns_number_total             12319
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202325h_si_001.cif
_cod_data_source_block           tx83
_cod_database_code               4328376