Chiral carbene-borane adducts: precursors for borenium catalysts for asymmetric FLP hydrogenations.
Lam, Jolie; Günther, Benjamin A R; Farrell, Jeffrey M.; Eisenberger, Patrick; Bestvater, Brian P.; Newman, Paul D.; Melen, Rebecca L.; Crudden, Cathleen M.; Stephan, Douglas W.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 15303–; doi:10.1039/c6dt02202b

data_7039630
_publ_section_title
;
 Chiral carbene-borane adducts: precursors for borenium catalysts for
 asymmetric FLP hydrogenations.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15303
_journal_paper_doi               10.1039/c6dt02202b
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C21 H38 B N2, B C24 F20'
_chemical_formula_sum            'C45 H38 B2 F20 N2'
_chemical_formula_weight         1008.43
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_Int_Tables_number      1
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_audit_creation_date             2016-01-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-05-26 deposited with the CCDC.
2016-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                103.359(5)
_cell_angle_beta                 99.814(5)
_cell_angle_gamma                111.620(5)
_cell_formula_units_Z            2
_cell_length_a                   12.4169(13)
_cell_length_b                   12.4961(14)
_cell_length_c                   15.9381(17)
_cell_measurement_reflns_used    9133
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.36
_cell_volume                     2145.7(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      149.93
_diffrn_measured_fraction_theta_full 0.9172
_diffrn_measured_fraction_theta_max 0.8918
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41777
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.37
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.151
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0679 before and 0.0495 after correction.
The Ratio of minimum to maximum transmission is 0.9134.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.5607
_exptl_crystal_description       block
_exptl_crystal_F_000             1024.9307
_refine_diff_density_max         0.3017
_refine_diff_density_min         -0.2798
_refine_diff_density_rms         0.0604
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.2(4)
_refine_ls_d_res_high            0.7690
_refine_ls_d_res_low             14.8749
_refine_ls_goodness_of_fit_ref   1.0425
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    112
_refine_ls_number_parameters     1252
_refine_ls_number_reflns         17623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0425
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0635P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1100
_reflns_Friedel_coverage         0.813
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              20
_reflns_limit_l_min              -20
_reflns_number_gt                13697
_reflns_number_total             17623
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6dt02202b2.cif
_cod_data_source_block           BG002_0m
_cod_depositor_comments
'Adding full bibliography for 7039626--7039633.cif.'
_cod_original_sg_symbol_Hall     ' P 1'
_cod_database_code               7039630
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C54(H54), C62(H62), C66(H66), C78(H78), C140(H140), C148(H148)
2.b Secondary CH2 refined with riding coordinates:
 C50(H50a,H50b), C52(H52a,H52b), C55(H55a,H55b), C57(H57a,H57b), C63(H63a,
 H63b), C64(H64a,H64b), C65(H65a,H65b), C67(H67a,H67b), C68(H68a,H68b),
 C69(H69a,H69b), C71(H71a,H71b), C73(H73a,H73b), C76(H76a,H76b), C79(H79a,H79b),
  C141(H14a,H14b), C143(H14c,H14d), C144(H14e,H14f), C145(H14g,H14h), C146(H14i,
 H14j), C147(H14k,H14l)
2.c Idealised Me refined as rotating group:
 C1aa(H1aa,H1ab,H1ac), C51(H51a,H51b,H51c), C53(H53a,H53b,H53c), C56(H56a,H56b,
 H56c), C60(H60a,H60b,H60c), C31(H31a,H31b,H31c), C72(H72a,H72b,H72c), C74(H74a,
 H74b,H74c), C80(H80a,H80b,H80c), C139(H13a,H13b,H13c)
;
_olex2_submission_special_instructions 'No special instructions were received'