The carboboration of Me3Si-substituted alkynes and allenes with boranes and borocations.
Lawson, James R.; Fasano, Valerio; Cid, Jessica; Vitorica-Yrezabal, Inigo; Ingleson, Michael J.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 6060–6070; doi:10.1039/c5dt03003j

data_7036439
_publ_section_title
;
 The carboboration of Me3Si-substituted alkynes and allenes with boranes
 and borocations.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6060
_journal_page_last               6070
_journal_paper_doi               10.1039/c5dt03003j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C23 H30 B Br O2 Si'
_chemical_formula_sum            'C23 H30 B Br O2 Si'
_chemical_formula_weight         457.28
_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     direct
_audit_creation_date             2015-08-26
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_audit_update_record
;
2015-08-27 deposited with the CCDC.
2015-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.161(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5585(7)
_cell_length_b                   18.4820(8)
_cell_length_c                   12.0048(9)
_cell_measurement_reflns_used    2300
_cell_measurement_temperature    150.02(10)
_cell_measurement_theta_max      26.3130
_cell_measurement_theta_min      3.5700
_cell_volume                     2321.2(3)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies (2013)'
_computing_data_collection       'CrysAlisPro, Agilent Technologies (2013)'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies (2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.02(10)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.824
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.824
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8379
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.824
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.979
_diffrn_reflns_theta_min         3.410
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.838
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.95794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
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    1.309
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5079
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+3.5971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1343
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3511
_reflns_number_total             5079
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03003j2.cif
_cod_data_source_block           amji272
_cod_depositor_comments
'Adding full bibliography for 7036438--7036439.cif.'
_cod_database_code               7036439
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C205-C206
 2.4 with sigma of 0.02
 C105-C106
 2.4 with sigma of 0.02
 C106-C102
 2.4 with sigma of 0.02
 C102-C105
 2.4 with sigma of 0.02
 C104-C103
 2.4 with sigma of 0.02
 C107-C103
 2.4 with sigma of 0.02
 C104-C103
 2.4 with sigma of 0.02
 C107-C103
 2.4 with sigma of 0.02
 C206-C202
 2.4 with sigma of 0.02
 C205-C202
 2.4 with sigma of 0.02
 C207-C203
 2.4 with sigma of 0.02
 C204-C203
 2.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C203 \\sim O101: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
4. Rigid body (RIGU) restrains
 O100, O101, C202, C207, C205, C204, C206, C203
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O201, O200, C102, C104, C107, C106, C103, C105
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C205)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C202)=Sof(C203)=Sof(C206)=
 Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C204)=Sof(H20G)=Sof(H20H)=Sof(H20I)=
 Sof(O100)=Sof(O101)=Sof(C207)=Sof(H20J)=Sof(H20K)=Sof(H20L)=1-FVAR(1)
 Sof(C104)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C102)=Sof(C103)=Sof(C107)=
 Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C105)=Sof(H10G)=Sof(H10H)=Sof(H10I)=
 Sof(O200)=Sof(O201)=Sof(C106)=Sof(H10J)=Sof(H10K)=Sof(H10L)=FVAR(1)
6.a Me refined with riding coordinates:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C104(H10A,H10B,
 H10C), C205(H20A,H20B,H20C), C107(H10D,H10E,H10F), C206(H20D,H20E,H20F),
 C105(H10G,H10H,H10I), C204(H20G,H20H,H20I), C106(H10J,H10K,H10L), C207(H20J,
 H20K,H20L)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C13(H13), C14(H14)
;
_shelx_res_checksum              85979
_olex2_submission_special_instructions 'No special instructions were received'