Cluster Expansion Reactions of Group 6 Metallaboranes. Syntheses, Crystal Structures, and Spectroscopic Characterizations of (Cp*Cr)2B5H9, (Cp*Cr)2B4H8Fe(CO)3, (Cp*Cr)2B4H7Co(CO)3, and (Cp*Mo)2B5H9Fe(CO)3
Simon Aldridge; Hisako Hashimoto; Kazumori Kawamura; Maoyu Shang; Thomas P. Fehlner; Inorganic Chemistry 37 (1998) 928–940; doi:10.1021/ic971251k

data_4322691
_publ_section_title
;
 Cluster Expansion Reactions of Group 6 Metallaboranes. Syntheses, Crystal
 Structures, and Spectroscopic Characterizations of (Cp*Cr)2B5H9,
 (Cp*Cr)2B4H8Fe(CO)3, (Cp*Cr)2B4H7Co(CO)3, and (Cp*Mo)2B5H9Fe(CO)3
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              928
_journal_page_last               940
_journal_paper_doi               10.1021/ic971251k
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C20 H39 B5 Cr2'
_chemical_formula_weight         437.56
_chemical_name_systematic
; 
 (Me5CpCr)2B5H9
;
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_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            8
_cell_length_a                   23.711(2)
_cell_length_b                   23.711(2)
_cell_length_c                   8.4380(4)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     4743.9(6)
_computing_cell_refinement       'MADNES (Messerschmitt & Pflugrath, 1987)'
_computing_data_collection       'MADNES (Messerschmitt & Pflugrath, 1987)'
_computing_data_reduction        'MADNES (Messerschmitt & Pflugrath, 1987)'
_computing_molecular_graphics    'SHELXTL_V5 (Siemens, 1994)'
_computing_publication_material  'SHELXTL_V5 (Siemens, 1994)'
_computing_structure_refinement  'SHELXTL_V5 (Siemens, 1994)'
_computing_structure_solution    'SHELXTL_V5 (Siemens, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius FAST area-detector'
_diffrn_measurement_method       'ellipsoid-mask fitting'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0788
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            29246
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.43
_diffrn_standards_decay_%        'no measurable decay'
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.919
_exptl_absorpt_correction_T_max  0
_exptl_absorpt_correction_T_min  0
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_meas      ?
_exptl_crystal_description       bar-shaped
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.103
_refine_ls_goodness_of_fit_obs   1.194
_refine_ls_hydrogen_treatment
' refall for borane group, with riding model for methyl ones'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5503
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.103
_refine_ls_restrained_S_obs      1.194
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_obs          0.0652
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+5.9896P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1680
_refine_ls_wR_factor_obs         0.1484
_reflns_number_observed          3724
_reflns_number_total             5503
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971251k_3.cif
_cod_data_source_block           C20H39B5Cr2
_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^)+(0.0608P)^2^+5.9896P] 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^)+(0.0608P)^2^+5.9896P] 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        4744.0(7)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               4322691