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_4077765
_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            'C11 H22 B3 Ir O'
_chemical_formula_weight         394.92
_chemical_name_systematic
;

C5Me5Ir(CO)B3H7

;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.400(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.2512(4)
_cell_length_b                   14.4243(18)
_cell_length_c                   28.001(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      10
_cell_volume                     2904.3(6)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  '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  0.0225
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5239
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        '0.7086 - 1.0000'
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.171
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6476
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column-like
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.171
_refine_diff_density_min         -1.169
_refine_diff_density_rms         0.210
_refine_ls_extinction_method
;

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_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         5127
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+16.0591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1324
_reflns_number_gt                3665
_reflns_number_total             5127
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om990091c.cif
_cod_data_source_block           fe9817
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

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 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4077765