Synthesis and Structure of the Metallaborane Cp*3(μ-H)W3B8H8 from the Thermolysis of Cp*H3WB4H8 (Cp* = η5-C5Me5). A Close-Packed 11-Atom Boron-Rich Cluster
Andrew S. Weller; Maoyu Shang; Thomas P. Fehlner; Journal of the American Chemical Society 120 (1998) 8283–8284; doi:10.1021/ja981101o

data_4116808
_publ_section_title
;
 Synthesis and Structure of the Metallaborane Cp*3(\m-H)W3B8H8 from the
 Thermolysis of Cp*H3WB4H8 (Cp* = \h5-C5Me5). A Close-Packed 11-Atom
 Boron-Rich Cluster
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8283
_journal_page_last               8284
_journal_paper_doi               10.1021/ja981101o
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C30 H54 B8 W3'
_chemical_formula_weight         1052.76
_chemical_name_systematic
;

 (Me5CpW)3B8H9

;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.8507(13)
_cell_length_b                   14.1146(12)
_cell_length_c                   13.7229(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      15
_cell_volume                     3457.6(5)
_computing_cell_refinement       'CAD4-ARGUS (Enraf-Nonius, 1994)'
_computing_data_collection       'CAD4-ARGUS (Enraf-Nonius, 1994)'
_computing_data_reduction
;

Chi90s (Boyle, 1996), Xcad4 (Harms, 1996), SHELXTL-V5 (Siemens, 1994)

;
_computing_molecular_graphics
;
ORTEP-III (Farrugia, Burnett, Johnson, 1996)
;
_computing_publication_material  'SHELXTL-V5 (Siemens, 1994)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w/2\q
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3155
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.976
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4404
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.022
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.171
_refine_diff_density_min         -1.619
_refine_diff_density_rms         0.150
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_coef       0.00007(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.061
_refine_ls_goodness_of_fit_obs   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         3154
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.127
_refine_ls_restrained_S_obs      1.060
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_obs          0.0349
_refine_ls_shift/esd_max         0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+7.4516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1000
_refine_ls_wR_factor_obs         0.0929
_reflns_number_observed          3076
_reflns_number_total             3155
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja981101o.cif
_cod_data_source_block           fe9803
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+7.4516P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+7.4516P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4116808