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_4322690
_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            'C23 H39 B5 Fe Mo2 O3'
_chemical_formula_weight         665.32
_chemical_name_systematic
; 
(Me5CpMo)2B5H9Fe(CO)3
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   24.679(7)
_cell_length_b                   25.126(2)
_cell_length_c                   17.958(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      13
_cell_volume                     11135(4)
_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    'SHELXTL-V5 (Siemens, 1994)'
_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  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5060
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.31
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.424
_exptl_absorpt_correction_T_max  0.9901
_exptl_absorpt_correction_T_min  0.9600
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle-shaped
_exptl_crystal_F_000             5376
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.045
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.41(4)
_refine_ls_goodness_of_fit_all   1.168
_refine_ls_goodness_of_fit_obs   1.173
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         4890
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.167
_refine_ls_restrained_S_obs      1.172
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_obs          0.0390
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+87.3747P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1009
_refine_ls_wR_factor_obs         0.0994
_reflns_number_observed          4718
_reflns_number_total             4890
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971251k_2.cif
_cod_data_source_block           f9703
_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^)+(0.0438P)^2^+87.3747P] 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^)+(0.0438P)^2^+87.3747P] 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        11135.3(34)
_cod_database_code               4322690