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_7122349
_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         'C11 H25 B9 N Na O5 S2'
_chemical_formula_sum            'C11 H25 B9 N Na O5 S2'
_chemical_formula_weight         435.72
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-04-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2018-07-10 deposited with the CCDC.
2018-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.3755(8)
_cell_length_b                   11.2861(6)
_cell_length_c                   51.571(3)
_cell_measurement_reflns_used    9527
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      53.91
_cell_measurement_theta_min      3.409
_cell_volume                     8367.1(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      170.0
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.1503
_diffrn_reflns_av_unetI/netI     0.1156
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_number            73033
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.138
_diffrn_reflns_theta_min         4.007
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.879
_exptl_absorpt_correction_T_max  0.7431
_exptl_absorpt_correction_T_min  0.4926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1919 before and 0.1338 after correction. The Ratio of minimum to maximum transmission is 0.6629. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.692
_exptl_crystal_description       block
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       0.0016(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         7759
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.1897
_refine_ls_R_factor_gt           0.1650
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+82.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3796
_refine_ls_wR_factor_ref         0.3961
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5190
_reflns_number_total             7759
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05983g2.cif
_cod_data_source_block           wmj18026_0m
_cod_depositor_comments
'Adding full bibliography for 7122346--7122349.cif.'
_cod_database_code               7122349
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.933
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3-C5
 1.53 with sigma of 0.02
 C3-C4
 1.53 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C3(H3)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C6(H6), C7(H7), C9(H9), C10(H10)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C)
3.d Boron cage BH refined with riding coordinates:
 B2(H2), B3(H3A), B5(H5), B6(H6A), B7(H7A), B8(H8)
;
_shelx_res_checksum              80204
_shelx_fab_checksum              1448
_olex2_submission_special_instructions 'No special instructions were received'