Complete reductive cleavage of CO facilitated by highly electrophilic borocations
Liam D. Curless; Ewan R. Clark; Jessica Cid; Alessandro Del Grosso; Michael J. Ingleson; Chem.Commun. 51 (2015) 10903–; doi:10.1039/C5cc03504J

data_7117382
_publ_section_title
;
 Complete reductive cleavage of CO facilitated by highly electrophilic
 borocations
;
_journal_name_full               Chem.Commun.
_journal_page_first              10903
_journal_paper_doi               10.1039/C5cc03504J
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C24 B F20, C12 H32 B N2'
_chemical_formula_sum            'C36 H32 B2 F20 N2'
_chemical_formula_weight         894.25
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-01-08
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4957)
;
_audit_update_record
;
2015-04-09 deposited with the CCDC.
2015-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                82.373(4)
_cell_angle_beta                 83.288(4)
_cell_angle_gamma                81.661(4)
_cell_formula_units_Z            2
_cell_length_a                   8.7661(5)
_cell_length_b                   13.7257(7)
_cell_length_c                   15.8543(8)
_cell_measurement_reflns_used    3803
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.2120
_cell_measurement_theta_min      3.7500
_cell_volume                     1861.44(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9974
_diffrn_measured_fraction_theta_max 0.8534
_diffrn_measurement_details
;
  1 omega   32.00   90.00   1.0000    3.1750
omega____ theta____ kappa____ phi______ frames
    -       21.6485   57.0000  -60.0000 58

  2 omega    0.00   59.00   1.0000    3.1750
omega____ theta____ kappa____ phi______ frames
    -       21.6485   57.0000   30.0000 59

  3 omega   -2.00   89.00   1.0000    3.1750
omega____ theta____ kappa____ phi______ frames
    -       21.6485   57.0000 -150.0000 91

  4 omega   34.00   64.00   1.0000    3.1750
omega____ theta____ kappa____ phi______ frames
    -       21.6485  -99.0000   60.0000 30

  5 omega   17.00   66.00   1.0000    3.1750
omega____ theta____ kappa____ phi______ frames
    -       21.6485  -99.0000 -120.0000 49

  6 omega  -49.00   45.00   1.0000    3.1750
omega____ theta____ kappa____ phi______ frames
    -       21.6485  -57.0000   60.0000 94

  7 omega  -47.00  -19.00   1.0000    3.1750
omega____ theta____ kappa____ phi______ frames
    -       21.6485  -57.0000  150.0000 28
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0246115000
_diffrn_orient_matrix_UB_12      0.0465068000
_diffrn_orient_matrix_UB_13      -0.0229441000
_diffrn_orient_matrix_UB_21      -0.0360824000
_diffrn_orient_matrix_UB_22      0.0174326000
_diffrn_orient_matrix_UB_23      0.0385805000
_diffrn_orient_matrix_UB_31      0.0696204000
_diffrn_orient_matrix_UB_32      0.0173060000
_diffrn_orient_matrix_UB_33      0.0065530000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0747
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.853
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14253
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.853
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.898
_diffrn_reflns_theta_min         3.337
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82354
_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            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_description       irregular
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         8377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+0.7581P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1126
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5505
_reflns_number_total             8377
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc03504j2.cif
_cod_data_source_block           amji226
_cod_database_code               7117382
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         C18H22B1F20N1
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H3A(0.037) H3B(0.037) H5A(0.033) H5B(0.033) H2A(0.047) H2B(0.047)
 H2C(0.047) H7A(0.029) H7B(0.029) H8A(0.047) H8B(0.047) H8C(0.047) H11A(0.031)
 H11B(0.031) H1A(0.031) H1B(0.031) H9A(0.028) H9B(0.028) H4A(0.056) H4B(0.056)
 H4C(0.056) H10A(0.043) H10B(0.043) H10C(0.043) H6A(0.058) H6B(0.058)
 H6C(0.058) H12A(0.048) H12B(0.048) H12C(0.048)
 Fixed X: H3A(0.6474) H3B(0.683) H5A(0.5542) H5B(0.4771) H2A(0.4221)
 H2B(0.4386) H2C(0.273) H7A(0.115) H7B(0.0499) H8A(0.135) H8B(0.015)
 H8C(0.1967) H11A(0.1692) H11B(0.2587) H1A(0.2853) H1B(0.2683) H9A(0.4129)
 H9B(0.3204) H4A(0.4968) H4B(0.4672) H4C(0.6322) H10A(0.1835) H10B(0.0875)
 H10C(0.2137) H6A(0.7342) H6B(0.7103) H6C(0.786) H12A(0.3978) H12B(0.4967)
 H12C(0.3807)
 Fixed Y: H3A(0.243) H3B(0.1609) H5A(0.3896) H5B(0.3721) H2A(0.4103)
 H2B(0.3108) H2C(0.3763) H7A(0.2498) H7B(0.1988) H8A(0.0409) H8B(0.1048)
 H8C(0.093) H11A(0.2985) H11B(0.3476) H1A(0.2382) H1B(0.3374) H9A(0.1115)
 H9B(0.0461) H4A(0.0692) H4B(0.1506) H4C(0.0838) H10A(0.167) H10B(0.1049)
 H10C(0.0484) H6A(0.3751) H6B(0.2608) H6C(0.3004) H12A(0.2591) H12B(0.2961)
 H12C(0.3744)
 Fixed Z: H3A(0.3937) H3B(0.3292) H5A(0.3005) H5B(0.2183) H2A(0.4112)
 H2B(0.4765) H2C(0.4695) H7A(0.2877) H7B(0.217) H8A(0.2875) H8B(0.3495)
 H8C(0.3591) H11A(0.116) H11B(0.1781) H1A(0.3959) H1B(0.3309) H9A(0.1097)
 H9B(0.1835) H4A(0.4129) H4B(0.4786) H4C(0.4678) H10A(0.0443) H10B(0.1195)
 H10C(0.0553) H6A(0.1745) H6B(0.1818) H6C(0.2556) H12A(0.0305) H12B(0.0959)
 H12C(0.042)
;
_olex2_submission_special_instructions 'No special instructions were received'