Utilization of Transition-Metal Properties To Control Polyborane Formation. Synthesis of the arachno-Diiridahexaborane(12) 2,5-{Cp*IrH}2B4H8 and Its Conversion to the nido-Diiridahexaborane(10) 1,2-{Cp*Ir}2(-H)B4H7 (Cp* =5-C5Me5)
Xinjian Lei; Maoyu Shang; Thomas P. Fehlner; Organometallics 19 (2000) 118–120; doi:10.1021/om990816c

data_4063213
_publ_section_title
;
 Utilization of Transition-Metal Properties To Control Polyborane
 Formation. Synthesis of the arachno-Diiridahexaborane(12)
 2,5-{Cp*IrH}2B4H8 and Its Conversion to the nido-Diiridahexaborane(10)
 1,2-{Cp*Ir}2(-H)B4H7 (Cp* \\db 5-C5Me5)
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_journal_name_full               Organometallics
_journal_page_first              118
_journal_page_last               120
_journal_paper_doi               10.1021/om990816c
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C20 H40 B4 Ir2'
_chemical_formula_weight         708.16
_chemical_name_systematic
;

{(C5Me5)Ir2B4H10

;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 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            4
_cell_length_a                   8.7599(7)
_cell_length_b                   8.7599(7)
_cell_length_c                   30.4203(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      15
_cell_volume                     2334.3(3)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1992)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1992)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'ORTEP-III for Windows (Farrugia,1997)'
_computing_publication_material  'SHELXTL-V5 (Siemens Inc. 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       'non-profiled omega 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2054
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.42
_diffrn_standards_decay_%        0.9576-1.0223
_diffrn_standards_interval_count 250
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    11.392
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.332
_exptl_absorpt_correction_type   XABS2
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.015
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'square pyramid'
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.082
_refine_diff_density_min         -1.208
_refine_diff_density_rms         0.208
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.112
_refine_ls_goodness_of_fit_obs   1.132
_refine_ls_hydrogen_treatment
;

idealized with riding models for C5Me5 groups and other hydrogen atoms were

located from Difference Fourier map and refined with bond lengthen constraint

;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         2053
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.115
_refine_ls_restrained_S_obs      1.130
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_obs          0.0429
_refine_ls_shift/esd_max         -0.029
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+4.3097P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1003
_refine_ls_wR_factor_obs         0.0968
_reflns_number_observed          1873
_reflns_number_total             2054
_reflns_observed_criterion       >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+4.3097P] 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^)+(0.0529P)^2^+4.3097P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P4(1)2(1)2
_cod_database_code               4063213