Ruthenium, Rhodium, and Iridium Bis(σ-B−H) Diisopropylaminoborane Complexes†
Alcaraz, Gilles; Chaplin, Adrian B.; Stevens, Charlotte J.; Clot, Eric; Vendier, Laure; Weller, Andrew S.; Sabo-Etienne, Sylviane; Organometallics 29 (2010) 5591–; doi:10.1021/om1004995

data_4066505
_publ_section_title
;
 Ruthenium, Rhodium, and Iridium Bis(\s-B&#x2212;H) Diisopropylaminoborane
 Complexes&#x2020;
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5591
_journal_paper_doi               10.1021/om1004995
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety
'2(C36 H62 Ir P2), 2(C32 H12 B F24), 1.5(C6 H5 F)'
_chemical_formula_sum            'C145 H155.5 B2 F49.5 Ir2 P4'
_chemical_formula_weight         3368.59
_chemical_melting_point          ?
_chemical_name_common            'Compound A'
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.4772(4)
_cell_angle_beta                 96.9176(4)
_cell_angle_gamma                99.6400(4)
_cell_formula_units_Z            2
_cell_length_a                   13.05100(10)
_cell_length_b                   19.5769(2)
_cell_length_c                   28.2597(3)
_cell_measurement_reflns_used    21844
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      5.097
_cell_volume                     7063.53(12)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_sigmaI/netI    0.1049
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            41612
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         5.11
_exptl_absorpt_coefficient_mu    2.043
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3390
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.254
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2067
_refine_ls_number_reflns         28449
_refine_ls_number_restraints     1506
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0883
_reflns_number_gt                18596
_reflns_number_total             28449
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1004995_si_002.cif
_cod_data_source_block           146abc10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_symmetry_cell_setting' value
'Triclinic' changed to 'triclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

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 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C145 H155.50 B2 F49.50 Ir2 P4'
_cod_database_code               4066505