Synthesis and Structure of {η5-C5H5Cr}2{μ-η6:η6-(μ-1,2-C3H6-1,2-C2B4H4)}. An Unusual 24-Electron Triple-Decker Sandwich Complex Containing a Metal-Stabilized, Planar Tetraborabenzene
Kazumori Kawamura; Maoyu Shang; Olaf Wiest; Thomas P. Fehlner; Inorganic Chemistry 37 (1998) 608–609; doi:10.1021/ic9712784

data_4322658
_publ_section_title
;
 Synthesis and Structure of
 {\h5-C5H5Cr}2{\m-\h6:\h6-(\m-1,2-C3H6-1,2-C2B4H4)}. An Unusual
 24-Electron Triple-Decker Sandwich Complex Containing a Metal-Stabilized,
 Planar Tetraborabenzene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              608
_journal_page_last               609
_journal_paper_doi               10.1021/ic9712784
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C15 H20 B4 Cr2'
_chemical_formula_weight         347.55
_chemical_name_systematic
; 
 {eta5-C5H5Cr}2{mu-eta6:eta6-(mu-1,2-C3H6-1,2-C2B4H4)} 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 109.46(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.820(3)
_cell_length_b                   9.836(2)
_cell_length_c                   14.471(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      13
_cell_volume                     1586.3(7)
_computing_cell_refinement       'CAD4 (Enraf-Nonius, 1977)'
_computing_data_collection       'CAD4 (Enraf-Nonius, 1977)'
_computing_data_reduction        'SDP_Package (Enraf-Nonius, 1985)'
_computing_molecular_graphics    'ORTEP-III (Burnett & Jognson, 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       \q/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  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2929
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.55
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.354
_exptl_absorpt_correction_T_max  0.9990
_exptl_absorpt_correction_T_min  0.8414
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle-like
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.121
_refine_ls_goodness_of_fit_obs   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         2785
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.121
_refine_ls_restrained_S_obs      1.102
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_obs          0.0464
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+1.4279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1220
_refine_ls_wR_factor_obs         0.0984
_reflns_number_observed          1939
_reflns_number_total             2786
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9712784.cif
_cod_data_source_block           f9712
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+1.4279P] 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^)+(0.0411P)^2^+1.4279P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1586.4(7)
_cod_database_code               4322658