Synthesis of Iridaboratranes Bearing Phosphine-Tethered Borane: Reversible CO/PR3(R = Me, OMe, OEt) Substitution Reactions Induced by a σ-Electron-Acceptor Borane Ligand
Kameo, Hajime; Hashimoto, Yasuhiro; Nakazawa, Hiroshi; Organometallics 31 (2012) 4251–; doi:10.1021/om300216g

data_4078459
_publ_section_title
;
 Synthesis of Iridaboratranes Bearing Phosphine-Tethered Borane:
 Reversible CO/PR3(R = Me, OMe, OEt) Substitution Reactions Induced by a
 \s-Electron-Acceptor Borane Ligand
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              4251
_journal_paper_doi               10.1021/om300216g
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C55 H43 B Ir O P3, C4 H8 O, 0.5(C12 H24 O6)'
_chemical_formula_sum            'C65 H63 B Ir O5 P3'
_chemical_formula_weight         1220.07
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 123.705(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.684(3)
_cell_length_b                   21.3585(17)
_cell_length_c                   21.512(2)
_cell_measurement_reflns_used    10634
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      4.0191
_cell_volume                     11346.1(19)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2001)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 7.32
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
scan:
    Number of images: 1800
               Slice: -80.0000 - 100.0000
         Image width: 0.1000
            Exp time: 18.0000
       Rotation axis: Phi
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 55.3295
              2theta: 24.7030
scan:
    Number of images: 600
               Slice: -15.0000 - 45.0000
         Image width: 0.1000
            Exp time: 18.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 0.0000
                 XTD: 55.3295
              2theta: 24.7030
scan:
    Number of images: 600
               Slice: -15.0000 - 45.0000
         Image width: 0.1000
            Exp time: 18.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 90.0000
                 XTD: 55.3295
              2theta: 24.7030
scan:
    Number of images: 600
               Slice: -15.0000 - 45.0000
         Image width: 0.1000
            Exp time: 18.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 180.0000
                 XTD: 55.3295
              2theta: 24.7030
scan:
    Number of images: 600
               Slice: -15.0000 - 45.0000
         Image width: 0.1000
            Exp time: 18.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 270.0000
                 XTD: 55.3295
              2theta: 24.7030

;
_diffrn_measurement_device       'Mercury CCD (2x2 bin mode)'
_diffrn_measurement_device_details 'AFC7: Eulerian 3-circle'
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       '\w or \f'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0897
_diffrn_reflns_av_sigmaI/netI    0.0839
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39953
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         4.05
_diffrn_source_current           250.0000
_diffrn_source_power             15.0000
_diffrn_source_voltage           60.0000
_exptl_absorpt_coefficient_mu    2.488
_exptl_absorpt_correction_T_max  0.8651
_exptl_absorpt_correction_T_min  0.8258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4960
_exptl_crystal_preparation
'mounted on the CryoLoop with Palaton oil and placed in N2 stream at 200(2) K'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.348
_refine_diff_density_min         -1.943
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         11538
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.1241
_refine_ls_R_factor_gt           0.0972
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+364.4679P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1870
_refine_ls_wR_factor_ref         0.2007
_reflns_number_gt                9141
_reflns_number_total             11538
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300216g_si_002.cif
_cod_data_source_block           1-Ir
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        11346(2)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4078459