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_7117381
_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         'B C24 F20, C13 H35 B2 N2 O'
_chemical_formula_sum            'C37 H35 B3 F20 N2 O'
_chemical_formula_weight         936.10
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.19 svn.r3143 for OlexSys, GUI svn.r4992)
;
_audit_update_record
;
2015-04-09 deposited with the CCDC.
2015-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.982(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3212(4)
_cell_length_b                   15.0201(6)
_cell_length_c                   17.8636(6)
_cell_measurement_temperature    293(2)
_cell_volume                     4060.5(2)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17318
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.26
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.155
_exptl_absorpt_correction_type   none
_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    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         8287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1505
_refine_ls_wR_factor_ref         0.1792
_reflns_number_gt                5637
_reflns_number_total             8287
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc03504j2.cif
_cod_data_source_block           amji222red
_cod_database_code               7117381
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H7A(0.051) H7B(0.051) H11A(0.17) H11B(0.17) H11C(0.17) H21A(0.1)
 H21B(0.1) H21C(0.1) H1AA(0.083) H1AB(0.083) H1AC(0.083) H29A(0.074)
 H29B(0.074) H31A(0.235) H31B(0.235) H31C(0.235) H38A(0.123) H38B(0.123)
 H38C(0.123) H0AA(0.058) H0AB(0.058) H24A(0.098) H24B(0.098) H24C(0.098)
 H49A(0.101) H49B(0.101) H49C(0.101) H56A(0.056) H56B(0.056) H58A(0.058)
 H58B(0.058) H70A(0.091) H70B(0.091)
 Fixed X: H7A(0.3978) H7B(0.4232) H11A(0.039) H11B(0.1313) H11C(0.0493)
 H21A(0.2995) H21B(0.3362) H21C(0.2362) H1AA(0.2788) H1AB(0.3336) H1AC(0.2618)
 H29A(0.0722) H29B(-0.0165) H31A(-0.068) H31B(-0.0637) H31C(-0.0434)
 H38A(0.0174) H38B(0.0365) H38C(0.1133) H0AA(0.4648) H0AB(0.4306) H24A(0.3614)
 H24B(0.4333) H24C(0.3697) H49A(0.3758) H49B(0.3455) H49C(0.4443) H56A(0.2475)
 H56B(0.2141) H58A(-0.0308) H58B(0.0468) H70A(0.0911) H70B(0.0839)
 Fixed Y: H7A(0.8345) H7B(0.8147) H11A(0.7848) H11B(0.7918) H11C(0.8414)
 H21A(0.8218) H21B(0.73) H21C(0.7536) H1AA(0.8593) H1AB(0.9372) H1AC(0.8878)
 H29A(0.7164) H29B(0.7048) H31A(0.5138) H31B(0.5911) H31C(0.493) H38A(0.5115)
 H38B(0.4679) H38C(0.513) H0AA(0.6739) H0AB(0.6771) H24A(0.6497) H24B(0.687)
 H24C(0.7526) H49A(0.5483) H49B(0.5506) H49C(0.53) H56A(0.6573) H56B(0.7498)
 H58A(0.6055) H58B(0.65) H70A(0.5633) H70B(0.4942)
 Fixed Z: H7A(0.5587) H7B(0.4786) H11A(0.2684) H11B(0.3202) H11C(0.343)
 H21A(0.631) H21B(0.6637) H21C(0.6617) H1AA(0.4237) H1AB(0.4664) H1AC(0.5046)
 H29A(0.4161) H29B(0.3604) H31A(0.3473) H31B(0.4067) H31C(0.434) H38A(0.1738)
 H38B(0.2545) H38C(0.2197) H0AA(0.5198) H0AB(0.598) H24A(0.3311) H24B(0.3955)
 H24C(0.3451) H49A(0.486) H49B(0.5659) H49C(0.5592) H56A(0.563) H56B(0.5298)
 H58A(0.2591) H58B(0.2256) H70A(0.4401) H70B(0.3738)
;
_olex2_submission_special_instructions 'No special instructions were received'