Oxidation Chemistry of Axially Protected Mo2 and W2 Quadruply Bonded Compounds
Michael Nippe; Eric Victor; John F. Berry; Inorganic Chemistry 48 (2009) 11889–11895; doi:10.1021/ic901965b

data_4303932
_publ_section_title
;
Oxidation Chemistry of Axially Protected Mo2 and W2 Quadruply Bonded Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11889
_journal_page_last               11895
_journal_paper_doi               10.1021/ic901965b
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C40 H32 N12 W2, C24 H20 B'
_chemical_formula_sum            'C64 H52 B N12 W2'
_chemical_formula_weight         1367.67
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 122.096(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.648(4)
_cell_length_b                   18.568(4)
_cell_length_c                   16.291(3)
_cell_measurement_reflns_used    7237
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.5137
_cell_measurement_theta_min      2.5619
_cell_volume                     5291.2(18)
_computing_cell_refinement       'SAINT Ver. 6.22  (Bruker-AXS, 2003)'
_computing_data_collection       'SMART Ver. 5.622 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT Ver. 6.22'
_computing_molecular_graphics    'SHELXTL Ver. 6.14'
_computing_publication_material  'SHELXTL Ver. 6.14'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Bruker CCD-1000 area detector'
_diffrn_measurement_method       '0.30\% \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  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34137
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.51
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    4.400
_exptl_absorpt_correction_T_max  0.3324
_exptl_absorpt_correction_T_min  0.2856
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2692
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.32
_refine_diff_density_max         2.243
_refine_diff_density_min         -1.828
_refine_diff_density_rms         0.270
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         6931
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+6.1508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0727
_reflns_number_gt                6067
_reflns_number_total             6931
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901965b_si_001_2.cif
_cod_data_source_block           1BPh4(C2/c)
_cod_original_cell_volume        5291.3(19)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4303932