Synthesis and structures of anionic rhenium polyhydride complexes of boron‒hydride ligands and their application in catalysis
Donnelly, Liam J.; Parsons, Simon; Morrison, Carole A.; Thomas, Stephen P.; Love, Jason B.; Chemical Science  (2020) –; doi:10.1039/D0SC03458D

data_1559029
_publ_section_title
;
 Synthesis and structures of anionic rhenium polyhydride complexes of
 boron--hydride ligands and their application in catalysis
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC03458D
_journal_year                    2020
_chemical_formula_moiety         'C18 H43 B3 O6 Re, C16 H34 K O8'
_chemical_formula_sum            'C34 H77 B3 K O14 Re'
_chemical_formula_weight         967.68
_chemical_name_systematic        '[ReH7(Bpin)3][K(18c6)(DME)]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-08
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)

_shelx_SHELXL_version_number       '2018/3'

olomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.
Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.
Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.

_publ_contact_author_address      'University of Edinburgh, Joseph Black Building, David Brewster Road, Edinburgh, EH9 3FJ' 
_publ_contact_author_email        'jason.love@ed.ac.uk, Stephen.Thomas@ed.ac.uk'
_publ_contact_author_name         'Liam J. Donnelly, Simon Parsons, Gary S. Nichol, Stephen P. Thomas* and Jason B. Love*'
_publ_contact_author_fax          ?
_publ_contact_author_phone        ?
_publ_requested_journal           ?
_publ_section_title               'Synthesis and Structures of Anionic Rhenium Boryl Polyhydrides and their Catalysis'
_publ_section_abstract            'The anionic rhenium boryl hydride complex, [ReH7(Bpin)3]-, has been synthesized by exhaustive deoxygenation of perrhenate (ReO4-) with HBpin. X-ray diffraction, NMR and IR spectroscopy analysis supports its structure as a polyhydridic Re centre with trigonal planar geometry with respect to the boryl ligands. This complex was applied in the catalytic hydroboration N-heteroaromatic substrates using [NR4][ReO4] as a precatalyst and in the stoichiometric C-H borylation of arenes. The reactivity of  [ReH7(Bpin)3]- was further explored through reactions with 9-BBN or PPh3 to produce the corresponding derivatized complexes. This work represent the first example for the synthesis of Re compounds bearing boron-centred ligands in the Re(III), Re(V) and Re(VII) oxidation states.'

;
_audit_update_record
;
2020-01-21 deposited with the CCDC.	2020-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.810(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7160(14)
_cell_length_b                   23.102(2)
_cell_length_c                   14.7725(15)
_cell_measurement_reflns_used    9443
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.07
_cell_measurement_theta_min      2.24
_cell_volume                     4678.6(8)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.812
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.812
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9312
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.812
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.489
_diffrn_reflns_theta_min         2.239
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.741
_exptl_absorpt_correction_T_max  0.429594
_exptl_absorpt_correction_T_min  0.322402
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 316995 reflections, Rint = 0.0922
 (96379 with I > 3sig(I), Rint = 0.0563)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       needle
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.578
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.053
_refine_diff_density_max         1.332
_refine_diff_density_min         -2.414
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         9312
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+100.0126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1304
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8605
_reflns_number_total             9312
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc03458d2.cif
_cod_data_source_block           twin4_hatomsmoved
_cod_database_code               1559029
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.300
_shelx_res_checksum              95348
_olex2_submission_special_instructions 'No special instructions were received'