B-H functionalization of the monocarba-closo-dodecaborate anion by rhodium and iridium catalysis.
Shen, Yunjun; Pan, Yani; Zhang, Kang; Liang, Xuewei; Liu, Jiyong; Spingler, Bernhard; Duttwyler, Simon; Dalton transactions (Cambridge, England : 2003) 46 (2017) 3135–3140; doi:10.1039/c7dt00269f

data_7042024
_publ_section_title
;
 B-H functionalization of the monocarba-closo-dodecaborate anion by
 rhodium and iridium catalysis.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3135
_journal_page_last               3140
_journal_paper_doi               10.1039/c7dt00269f
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C20 H33 B11 N3 O5 S2, C8 H20 N, C3 H6 O'
_chemical_formula_sum            'C31 H59 B11 N4 O6 S2'
_chemical_formula_weight         766.85
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-04-08
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2015-10-28 deposited with the CCDC.
2017-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                118.275(6)
_cell_angle_beta                 95.886(5)
_cell_angle_gamma                96.271(4)
_cell_formula_units_Z            2
_cell_length_a                   13.0426(7)
_cell_length_b                   13.4923(7)
_cell_length_c                   13.9657(9)
_cell_measurement_reflns_used    3574
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.4842
_cell_measurement_theta_min      3.1862
_cell_volume                     2117.7(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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)
;
_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)
;
_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-97 (Sheldrick, 1990)'
_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_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0224182000
_diffrn_orient_matrix_UB_12      -0.0016229000
_diffrn_orient_matrix_UB_13      0.0475941000
_diffrn_orient_matrix_UB_21      0.0155190000
_diffrn_orient_matrix_UB_22      -0.0526348000
_diffrn_orient_matrix_UB_23      -0.0341560000
_diffrn_orient_matrix_UB_31      0.0484337000
_diffrn_orient_matrix_UB_32      0.0301621000
_diffrn_orient_matrix_UB_33      0.0007648000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0649
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13269
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.19
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76973
_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    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         7725
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0610
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0771P)^2^+0.5259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1499
_refine_ls_wR_factor_ref         0.1767
_reflns_number_gt                5170
_reflns_number_total             7725
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt00269f2.cif
_cod_data_source_block           141020_yjs_0054
_cod_depositor_comments
'Adding full bibliography for 7042023--7042033.cif.'
_cod_database_code               7042024
_chemical_oxdiff_formula         'c10 h10 n2 o8 B1 S1'
_reflns_odcompleteness_completeness 99.50
_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.a Riding coordinates:
 N1(H1), N2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C21(H21A,H21B), C23(H23A,
 H23B), C25(H25A,H25B), C27(H27A,H27B)
2.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C11(H11), C12(H12), C15(H15), C16(H16), C18(H18), C19(H19)
2.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,
 H31B,H31C)
2.e Boron cage BH refined with riding coordinates:
 B2(H2A), B4(H4), B5(H5), B6(H6), B7(H7), B8(H8A), B9(H9A), B10(H10), B11(H11A)
;