Facilitating access to the most easily ionized molecule: an improved synthesis of the key intermediate, W2(hpp)4Cl2, and related compounds.
Cotton, F. Albert; Donahue, James P.; Gruhn, Nadine E.; Lichtenberger, Dennis L.; Murillo, Carlos A.; Timmons, Daren J.; Van Dorn, Laura O.; Villagrán, Dino; Wang, Xiaoping; Inorganic chemistry 45 (2006) 201–213; doi:10.1021/ic0515709

data_4340251
_publ_section_title
;
 Facilitating access to the most easily ionized molecule: an improved
 synthesis of the key intermediate, W2(hpp)4Cl2, and related compounds.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              201
_journal_page_last               213
_journal_paper_doi               10.1021/ic0515709
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         '(C28 H48 N12 W2), 2(C32 H12 B F24)'
_chemical_formula_sum            'C92 H72 B2 F48 N12 W2'
_chemical_formula_weight         2646.94
_chemical_name_common            '[W2(hpp)4][TFPB]2'
_chemical_name_systematic
; 
 Bis(tetra(3,5-bis(trifluoromethyl)phenyl)borate)[W2(hpp)4]  
;
_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                87.365(2)
_cell_angle_beta                 88.944(2)
_cell_angle_gamma                76.617(2)
_cell_formula_units_Z            2
_cell_length_a                   13.2005(17)
_cell_length_b                   14.863(2)
_cell_length_c                   26.035(3)
_cell_measurement_reflns_used    8929
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.492
_cell_measurement_theta_min      2.239
_cell_volume                     4963.9(11)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker Smart 1000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            35427
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         1.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.459
_exptl_absorpt_correction_T_max  0.8467
_exptl_absorpt_correction_T_min  0.4939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2596
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.282
_refine_diff_density_min         -0.917
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1465
_refine_ls_number_reflns         22050
_refine_ls_number_restraints     812
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+14.1825P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.1054
_reflns_number_gt                17587
_reflns_number_total             22050
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0515709si20050914_104451.cif
_cod_data_source_block           cmpd6
_cod_original_cell_volume        4964.0(11)
_cod_database_code               4340251