Isolation of [Ru(IPr)2(CO)H]+ (IPr = 1,3-Bis(2,6-diisopropylphenyl)imidazol-2-ylidene) and Reactivity toward E‒H (E = H, B) Bonds
Riddlestone, Ian M.; McKay, David; Gutmann, Matthias J.; Macgregor, Stuart A.; Mahon, Mary F.; Sparkes, Hazel A.; Whittlesey, Michael K.; Organometallics 35 (2016) 1301–; doi:10.1021/acs.organomet.6b00173

data_4088553
_publ_section_title
;
 Isolation of [Ru(IPr)2(CO)H]+ (IPr =
 1,3-Bis(2,6-diisopropylphenyl)imidazol-2-ylidene) and Reactivity toward
 E--H (E = H, B) Bonds
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1301
_journal_paper_doi               10.1021/acs.organomet.6b00173
_journal_volume                  35
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_sum            'C93 H88 B2 F24 N4 O3 Ru'
_chemical_formula_weight         1888.4
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_method           'Jana2006 Version : 23/03/2015'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8189(1)
_cell_length_b                   19.5640(1)
_cell_length_c                   30.6463(2)
_cell_measurement_reflns_used    61920
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      71.8560
_cell_measurement_theta_min      3.9820
_cell_volume                     8884.88(9)
_computing_cell_refinement
;
For X-ray Analysis ONLY: CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
For X-ray Analysis ONLY: CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
For X-ray Analysis ONLY: CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    ORTEP
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement
;Petricek, V., Dusek, M. & Palatinus L. (2014). Z. Kristallogr. 229(5), 345-352.
Palatinus L. & Chapuis G. (2007). J. Appl. Cryst. 40, 786-790.
;
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Agilent Supernova and ISIS SXD'
_diffrn_radiation_probe          X-rays-AND-NEUTRONS
_diffrn_radiation_source         'X-ray tube and neutron source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_av_unetI/netI     0.0708
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            123490
_diffrn_reflns_theta_full        72.07
_diffrn_reflns_theta_max         72.07
_diffrn_reflns_theta_min         4.01
_diffrn_source                   'Agilent Supernova and ISIS SXD'
_exptl_absorpt_coefficient_mu    2.321
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70671
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.4118
_exptl_crystal_description       block
_exptl_crystal_F_000             3872
_exptl_crystal_size_max          0.1946
_exptl_crystal_size_mid          0.1810
_exptl_crystal_size_min          0.0979
_refine_diff_density_max         1.044
_refine_diff_density_min         -0.564
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.285(5)
_refine_ls_extinction_method     'none for X-Ray data'
_refine_ls_goodness_of_fit_ref   3.18
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1251
_refine_ls_number_reflns         17403
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0747
_refine_ls_shift/su_max          0.0016
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/(\s^2^(I)+0.0004I^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1605
_refine_ls_wR_factor_ref         0.1613
_reflns_number_gt                22891
_reflns_number_total             23576
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            om6b00173_si_003.cif
_cod_data_source_block           S14MKW23-X-RAY-AND-NEUTRON-REFINEMENT
_cod_original_sg_symbol_Hall     'P 2xab;2ybc;2zac'
_cod_original_formula_sum        'C93 H88 B2 F24 N4 O3 Ru1'
_cod_database_code               4088553