Rhodium(iii)-catalyzed dehydrogenative dialkenylation of the monocarba-closo-decaborate cluster by regioselective B-H activation.
Liang, Xuewei; Shen, Yunjun; Zhang, Kang; Liu, Jiyong; Duttwyler, Simon; Chemical communications (Cambridge, England) 54 (2018) 12451–12454; doi:10.1039/c8cc05983g

data_7122346
_publ_section_title
;
 Rhodium(iii)-catalyzed dehydrogenative dialkenylation of the
 monocarba-closo-decaborate cluster by regioselective B-H activation.
;
_journal_issue                   88
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12451
_journal_page_last               12454
_journal_paper_doi               10.1039/c8cc05983g
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C5 H17 B9 N O, C4 H10 N0.5, C4 N0.5'
_chemical_formula_sum            'C13 H27 B9 N2 O'
_chemical_formula_weight         324.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-06-22
_audit_creation_method
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Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
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_audit_update_record
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2018-07-10 deposited with the CCDC.
2018-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.864(19)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.845(4)
_cell_length_b                   10.2834(6)
_cell_length_c                   15.723(2)
_cell_measurement_reflns_used    2817
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.3648
_cell_measurement_theta_min      2.7843
_cell_volume                     4509.2(12)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -87.00    6.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4683  -38.0000  -30.0000 93

  2 omega  -63.00   22.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4683  -77.0000 -150.0000 85

  3 omega  -37.00   62.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4683   46.0000  135.0000 99
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0177359000
_diffrn_orient_matrix_UB_12      -0.0300390000
_diffrn_orient_matrix_UB_13      -0.0430021000
_diffrn_orient_matrix_UB_21      -0.0125291000
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_diffrn_orient_matrix_UB_23      0.0248384000
_diffrn_orient_matrix_UB_31      -0.0132489000
_diffrn_orient_matrix_UB_32      0.0589199000
_diffrn_orient_matrix_UB_33      -0.0136753000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13933
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.790
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.053
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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    0.956
_exptl_crystal_description       plate
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4123
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1195
_refine_ls_R_factor_gt           0.0823
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1721P)^2^+0.5426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2421
_refine_ls_wR_factor_ref         0.2862
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2517
_reflns_number_total             4123
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05983g2.cif
_cod_data_source_block           170622_lxw_1
_cod_depositor_comments
'Adding full bibliography for 7122346--7122349.cif.'
_cod_original_cell_volume        4509.1(12)
_cod_database_code               7122346
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'c10 h10 n2 o8 b1'
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.975
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B9-H9
 1.1 with sigma of 0.02
3. Others
 Fixed Sof: C10(0.5) C11(0.5) C12(0.5) C14(0.5)
4.a Ternary CH refined with riding coordinates:
 C3(H3)
4.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C8(H8A,H8B)
4.c Aromatic/amide H refined with riding coordinates:
 N1(H1)
4.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C0AA(H0AA,H0AB,H0AC), C7(H7A,H7B,H7C)
4.e Boron cage BH refined with riding coordinates:
 B1(H1A), B2(H2), B3(H3A), B4(H4), B5(H5), B6(H6), B7(H7), B8(H8)
;
_shelx_res_checksum              68364
_olex2_submission_special_instructions 'No special instructions were received'