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_7039629
_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         'C23 H43 B N2'
_chemical_formula_sum            'C23 H43 B N2'
_chemical_formula_weight         358.44
_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             2016-04-27
_audit_creation_method
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Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
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_audit_update_record
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2016-05-26 deposited with the CCDC.
2016-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                91.586(2)
_cell_angle_beta                 109.357(3)
_cell_angle_gamma                93.844(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4015(3)
_cell_length_b                   9.5499(3)
_cell_length_c                   12.9102(4)
_cell_measurement_reflns_used    8401
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.118
_cell_measurement_theta_min      4.067
_cell_volume                     1089.60(6)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_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    SHELXS
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.8116
_diffrn_measured_fraction_theta_max 0.8095
_diffrn_measurement_device_type  'Supernova Dual Atlas'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18560
_diffrn_reflns_theta_full        29.8735
_diffrn_reflns_theta_max         29.87
_diffrn_reflns_theta_min         3.35
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.979
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model. Empirical absorption correction using 
spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.0924
_exptl_crystal_description       block
_exptl_crystal_F_000             400.1232
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.2503
_refine_diff_density_min         -0.1856
_refine_diff_density_rms         0.0457
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0(3)
_refine_ls_d_res_high            0.7135
_refine_ls_d_res_low             6.0816
_refine_ls_goodness_of_fit_ref   1.0711
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    128
_refine_ls_number_parameters     483
_refine_ls_number_reflns         10164
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0711
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+0.2889P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1254
_reflns_Friedel_coverage         0.757
_reflns_limit_h_max              11
_reflns_limit_h_min              -12
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              17
_reflns_limit_l_min              -17
_reflns_number_gt                8977
_reflns_number_total             10164
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6dt02202b2.cif
_cod_data_source_block           rm1552
_cod_depositor_comments
'Adding full bibliography for 7039626--7039633.cif.'
_cod_original_sg_symbol_Hall     ' P 1'
_cod_database_code               7039629
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1(3) 0(3)
2. 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
3.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C11(H11), C14(H14), C17(H17), C32(H32), C33(H33),
 C37(H37), C41(H41), C44(H44), C47(H47)
3.b Secondary CH2 refined with riding coordinates:
 C4(H4a,H4b), C5(H5a,H5b), C6(H6a,H6b), C8(H8a,H8b), C9(H9a,H9b), C10(H10a,
 H10b), C18(H18a,H18b), C19(H19a,H19b), C34(H34a,H34b), C35(H35a,H35b),
 C36(H36a,H36b), C38(H38a,H38b), C39(H39a,H39b), C40(H40a,H40b), C48(H48a,H48b),
  C49(H49a,H49b)
3.c Idealised Me refined as rotating group:
 C12(H12a,H12b,H12c), C13(H13a,H13b,H13c), C15(H15a,H15b,H15c), C16(H16a,H16b,
 H16c), C22(H22a,H22b,H22c), C23(H23a,H23b,H23c), C24(H24a,H24b,H24c), C42(H42a,
 H42b,H42c), C43(H43a,H43b,H43c), C45(H45a,H45b,H45c), C46(H46a,H46b,H46c),
 C52(H52a,H52b,H52c), C53(H53a,H53b,H53c), C54(H54a,H54b,H54c)
;
_olex2_submission_special_instructions 'No special instructions were received'