Rapid Reversible Borane to Boryl Hydride Exchange by Metal Shuttling on the Carborane Cluster Surface
Eleazer, Bennett J.; Smith, Mark D.; Popov, Alexey A.; Peryshkov, Dmitry V.; Chem. Sci.  (2017) –; doi:10.1039/C7SC01846K

data_1546117
_publ_section_title
;
 Rapid Reversible Borane to Boryl Hydride Exchange by Metal Shuttling on
 the Carborane Cluster Surface
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC01846K
_journal_year                    2017
_chemical_formula_moiety         'C32 H53 B10 O2 P3 Ru'
_chemical_formula_sum            'C32 H53 B10 O2 P3 Ru'
_chemical_formula_weight         771.82
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-02-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-04-24 deposited with the CCDC.
2017-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                88.2590(10)
_cell_angle_beta                 81.9880(10)
_cell_angle_gamma                89.388(2)
_cell_formula_units_Z            4
_cell_length_a                   12.5744(5)
_cell_length_b                   15.5222(7)
_cell_length_c                   19.5052(8)
_cell_measurement_reflns_used    9978
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.07
_cell_measurement_theta_min      2.44
_cell_volume                     3768.1(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEXII v2014.9-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker PHOTON-100 area detector'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0898
_diffrn_reflns_av_unetI/netI     0.0734
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            82388
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.388
_diffrn_reflns_theta_max         26.388
_diffrn_reflns_theta_min         2.219
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  0.2065
_exptl_absorpt_correction_T_min  0.1822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0716 before and 0.0576 after correction.
The Ratio of minimum to maximum transmission is 0.8823.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       plate
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       0.00054(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     959
_refine_ls_number_reflns         15369
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+2.4275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0782
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11415
_reflns_number_total             15369
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc01846k2.cif
_cod_data_source_block           be2199
_cod_database_code               1546117
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.904
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C11A(H11A), C14A(H14A), C21A(H21A), C24A(H24A), C11B(H11B), C14B(H14B),
 C21B(H21B), C24B(H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C32A(H32A), C33A(H33A), C34A(H34A), C35A(H35A), C36A(H36A), C42A(H42A),
 C43A(H43A), C44A(H44A), C45A(H45A), C46A(H46A), C52A(H52A), C53A(H53A),
 C54A(H54A), C55A(H55A), C56A(H56A), C32B(H32B), C33B(H33B), C34B(H34B),
 C35B(H35B), C36B(H36B), C42B(H42B), C43B(H43B), C44B(H44B), C45B(H45B),
 C46B(H46B), C52B(H52B), C53B(H53B), C54B(H54B), C55B(H55B), C56B(H56B)
2.c Idealised Me refined as rotating group:
 C12A(H12D,H12E,H12F), C13A(H13D,H13E,H13F), C15A(H15D,H15E,H15F), C16A(H16D,
 H16E,H16F), C22A(H22D,H22E,H22F), C23A(H23D,H23E,H23F), C25A(H25D,H25E,H25F),
 C26A(H26D,H26E,H26F), C12B(H12A,H12B,H12C), C13B(H13A,H13B,H13C), C15B(H15A,
 H15B,H15C), C16B(H16A,H16B,H16C), C22B(H22A,H22B,H22C), C23B(H23A,H23B,H23C),
 C25B(H25A,H25B,H25C), C26B(H26A,H26B,H26C)
;
_shelx_res_checksum              37980
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id BE2199
_olex2_submission_special_instructions 'No special instructions were received'