Novel Iridaboranes from the Reactions of Cp*2Ir2HxCl4-x,x= 0−2, with LiBH4. Existence of a Concurrent Reaction Channel in the Conversion of Metal Chlorides to Metal Hydrides
Lei, Xinjian; Bandyopadhyay, Ananda K.; Shang, Maoyu; Fehlner, Thomas P.; Organometallics 18 (1999) 2294–; doi:10.1021/om990091c

data_4077766
_publ_section_title
;
 Novel Iridaboranes from the Reactions of Cp*2Ir2HxCl4-x,x= 0&#x2212;2,
 with LiBH4. Existence of a Concurrent Reaction Channel in the Conversion
 of Metal Chlorides to Metal Hydrides
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2294
_journal_paper_doi               10.1021/om990091c
_journal_volume                  18
_journal_year                    1999
_chemical_formula_sum            'C20 H38 B2 Ir2'
_chemical_formula_weight         684.52
_chemical_name_systematic
;

{(C5Me5Ir)2H3B2H5

;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                107.113(13)
_cell_angle_beta                 92.554(12)
_cell_angle_gamma                111.67(2)
_cell_formula_units_Z            2
_cell_length_a                   8.551(2)
_cell_length_b                   10.306(2)
_cell_length_c                   14.884(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      15
_cell_volume                     1147.5(4)
_computing_cell_refinement       'CAD4-ARGUS (Enraf-Nonius, 1994)'
_computing_data_collection       'CAD4-ARGUS (Enraf-Nonius, 1994)'
_computing_data_reduction
;

Chi90s (Boyle, 1997), Xcad4 (Harms, 1997),

SHELXTL-v5 (Siemens, 1994)

;
_computing_molecular_graphics    'ORTEP-III for Windows (Farrugia, 1997)'
_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
_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    0.0289
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4006
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.24
_diffrn_standards_decay_%        '0.7711 - 1.0002'
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    11.585
_exptl_absorpt_correction_T_max  0.63256
_exptl_absorpt_correction_T_min  0.49376
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.981
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block-like
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.743
_refine_diff_density_min         -2.196
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.058
_refine_ls_goodness_of_fit_obs   1.134
_refine_ls_hydrogen_treatment
;

B-H terminal hydrogen atoms and Hydride were located from the difmap

and refined isotropically with bond length constraint,

others idealized with riding models.

;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         4006
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.058
_refine_ls_restrained_S_obs      1.133
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_obs          0.0389
_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^)+(0.0636P)^2^+0.5468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1013
_refine_ls_wR_factor_obs         0.0963
_reflns_number_observed          3201
_reflns_number_total             4006
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om990091c.cif
_cod_data_source_block           fe0901
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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^)+(0.0636P)^2^+0.5468P] 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^)+(0.0636P)^2^+0.5468P] 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      P-1
_cod_database_code               4077766