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_4088552
_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_formula_moiety
'C55 H71 N4 O Ru, C32 H12 B F24, C3 H2.5 F0.5'
_chemical_formula_sum            'C96 H90.5 B F25.5 N4 O Ru'
_chemical_formula_weight         1912.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date
;
'Thu Oct 15 16:26:35 2015'
;
_audit_creation_method
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   43.3892(3)
_cell_length_b                   16.38469(11)
_cell_length_c                   12.67092(9)
_cell_measurement_reflns_used    65469
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      72.6780
_cell_measurement_theta_min      4.0360
_cell_volume                     9007.99(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2300
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            135955
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.747
_diffrn_reflns_theta_min         4.528
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.306
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)

Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       block
_exptl_crystal_F_000             3924
_exptl_crystal_size_max          0.1421
_exptl_crystal_size_mid          0.0877
_exptl_crystal_size_min          0.0551
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 7665 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0090(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1149
_refine_ls_number_reflns         17872
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+2.4849P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0633
_refine_ls_wR_factor_ref         0.0638
_reflns_Friedel_coverage         0.821
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                17519
_reflns_number_total             17872
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00173_si_003.cif
_cod_data_source_block           s15mkw37_sq
_cod_original_cell_volume        9008.00(11)
_cod_original_formula_sum        'C96 H90.50 B F25.50 N4 O Ru'
_cod_database_code               4088552