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_7042027
_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         'C38 H45 B11 F4 N O, C8 H20 N'
_chemical_formula_sum            'C46 H65 B11 F4 N2 O'
_chemical_formula_weight         856.91
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-03-12
_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                90.00
_cell_angle_beta                 99.089(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3433(7)
_cell_length_b                   25.3537(15)
_cell_length_c                   18.9697(13)
_cell_measurement_reflns_used    2927
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5379
_cell_measurement_theta_min      3.1223
_cell_volume                     4912.2(6)
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0170118000
_diffrn_orient_matrix_UB_12      -0.0238625000
_diffrn_orient_matrix_UB_13      -0.0186705000
_diffrn_orient_matrix_UB_21      -0.0131777000
_diffrn_orient_matrix_UB_22      -0.0118401000
_diffrn_orient_matrix_UB_23      0.0320030000
_diffrn_orient_matrix_UB_31      -0.0660257000
_diffrn_orient_matrix_UB_32      0.0085250000
_diffrn_orient_matrix_UB_33      -0.0078731000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_unetI/netI     0.0912
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19971
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.13
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94483
_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    1.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         8940
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1530
_refine_ls_R_factor_gt           0.0744
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1061P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1920
_refine_ls_wR_factor_ref         0.2466
_reflns_number_gt                4259
_reflns_number_total             8940
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt00269f2.cif
_cod_data_source_block           150311_yjs_0108
_cod_depositor_comments
'Adding full bibliography for 7042023--7042033.cif.'
_cod_database_code               7042027
_chemical_oxdiff_formula         'c10 h10 n2 o8 b1 f1'
_reflns_odcompleteness_completeness 99.60
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C6 \\sim C5 \\sim C4 \\sim C3: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C15(H15A,H15B), C16(H16A,
 H16B), C23(H23A,H23B), C24(H24A,H24B), C31(H31A,H31B), C32(H32A,H32B),
 C39(H39A,H39B), C41(H41A,H41B), C43(H43A,H43B), C45(H45A,H45B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7A), C8(H8), C10(H10A), C11(H11A), C13(H13), C14(H14), C18(H18), C19(H19),
  C21(H21), C22(H22), C26(H26), C27(H27), C29(H29), C30(H30), C34(H34),
 C35(H35), C37(H37), C38(H38)
3.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C46(H46A,H46B,
 H46C)
3.d Boron cage BH refined with riding coordinates:
 B2(H2), B6(H6), B7(H7), B8(H8A), B9(H9), B10(H10), B11(H11)
;