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_7036438
_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         'C36 H44 B5 Cl8 N8, 3(Al Cl4), C H2 Cl2'
_chemical_formula_sum            'C37 H46 Al3 B5 Cl22 N8'
_chemical_formula_weight         1517.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_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                 96.490(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.085(4)
_cell_length_b                   13.0664(19)
_cell_length_c                   23.157(6)
_cell_measurement_reflns_used    1163
_cell_measurement_temperature    150.02(10)
_cell_measurement_theta_max      19.9490
_cell_measurement_theta_min      3.3970
_cell_volume                     6640(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
  1 omega  -53.00   46.00   1.0000  170.0000
omega____ theta____ kappa____ phi______ frames
    -       -5.7757    0.0000  -30.0000 99

  2 omega    3.00   58.00   1.0000  170.0000
omega____ theta____ kappa____ phi______ frames
    -        6.3225   57.0000 -180.0000 55
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0008292000
_diffrn_orient_matrix_UB_12      -0.0271391000
_diffrn_orient_matrix_UB_13      0.0263269000
_diffrn_orient_matrix_UB_21      -0.0239821000
_diffrn_orient_matrix_UB_22      -0.0310725000
_diffrn_orient_matrix_UB_23      -0.0134993000
_diffrn_orient_matrix_UB_31      0.0216907000
_diffrn_orient_matrix_UB_32      -0.0352818000
_diffrn_orient_matrix_UB_33      -0.0086140000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.1245
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5396
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        18.846
_diffrn_reflns_theta_max         18.846
_diffrn_reflns_theta_min         3.080
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.979
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31164
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       needle
_exptl_crystal_F_000             3048
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         2585
_refine_ls_number_restraints     174
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1521
_refine_ls_R_factor_gt           0.0922
_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^)+(0.0822P)^2^+234.7403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2207
_refine_ls_wR_factor_ref         0.2559
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1587
_reflns_number_total             2585
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03003j2.cif
_cod_data_source_block           amji182
_cod_depositor_comments
'Adding full bibliography for 7036438--7036439.cif.'
_cod_database_code               7036438
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         C9H10N2B1Al1Cl5
_reflns_odcompleteness_completeness 98.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     18.81
_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. Uiso/Uaniso restraints and constraints
N13 \\sim N18 \\sim N15 \\sim N14: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004
C20 \\sim C22 \\sim C21 \\sim C23 \\sim C30 \\sim N14: within 2A with sigma of
0.002 and sigma for terminal atoms of 0.004
C34 \\sim B40 \\sim N13 \\sim C38 \\sim N18: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004
Uanis(C17) = Uanis(C31)
Uanis(B29) = Uanis(B35) = Uanis(B40)
Uanis(N13) = Uanis(N18) = Uanis(N15) = Uanis(N14)
3. Rigid body (RIGU) restrains
 C37, Cl33, Cl24
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C16, C17, C19, C20, C21, C22, C23, C25, C27, C28, C30, C31, C32, C34, C36,
 C37, C38, C1, C2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C1, N18, C16, C34, B40, N13, C38
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Fixed Sof: Cl24(0.5) Cl33(0.5) C37(0.5) H37A(0.5) H37B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B)
5.b Me refined with riding coordinates:
 C16(H16A,H16B,H16C), C27(H27A,H27B,H27C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
5.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C19(H19), C21(H21), C22(H22), C23(H23), C25(H25), C28(H28),
 C30(H30), C31(H31), C36(H36)
;
_shelx_res_checksum              12773
_olex2_submission_special_instructions 'No special instructions were received'