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_7042031
_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         'C26 H48 B11 Br N O9, C8 H20 N'
_chemical_formula_sum            'C34 H68 B11 Br N2 O9'
_chemical_formula_weight         847.72
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-06-14
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2016-10-28 deposited with the CCDC.
2017-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 129.407(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7123(11)
_cell_length_b                   18.5073(11)
_cell_length_c                   21.4306(19)
_cell_measurement_reflns_used    2944
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.4333
_cell_measurement_theta_min      2.9049
_cell_volume                     4815.1(7)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
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 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0243696000
_diffrn_orient_matrix_UB_12      -0.0092672000
_diffrn_orient_matrix_UB_13      -0.0372719000
_diffrn_orient_matrix_UB_21      0.0218892000
_diffrn_orient_matrix_UB_22      -0.0335349000
_diffrn_orient_matrix_UB_23      0.0001515000
_diffrn_orient_matrix_UB_31      -0.0315873000
_diffrn_orient_matrix_UB_32      -0.0160773000
_diffrn_orient_matrix_UB_33      0.0211047000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0736
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19449
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.22
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.900
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90143
_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    1.169
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         8676
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1663
_refine_ls_R_factor_gt           0.0834
_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^)+(0.1298P)^2^+2.0492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2160
_refine_ls_wR_factor_ref         0.2746
_reflns_number_gt                4243
_reflns_number_total             8676
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt00269f2.cif
_cod_data_source_block           160613_sd_1
_cod_depositor_comments
'Adding full bibliography for 7042023--7042033.cif.'
_cod_original_cell_volume        4815.1(6)
_cod_database_code               7042031
_chemical_oxdiff_formula         'c10 h10 n2 o7 Br1 b1'
_reflns_odcompleteness_completeness 99.49
_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. Restrained distances
 O9-C25
 1.53 with sigma of 0.02
 C25-C26
 1.53 with sigma of 0.02
 O7-C20
 1.53 with sigma of 0.02
 C20-C21
 1.53 with sigma of 0.02
 O9-C26
 2.53 with sigma of 0.04
 O7-C21
 2.53 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C22 \\sim O2 \\sim O3 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim O8 \\sim O9
\\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C3 \\sim C4 \\sim C5 \\sim C6
\\sim O6 \\sim O7 \\sim C18 \\sim C19 \\sim C20 \\sim C21: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
 C10(H10A,H10B), C12(H12A,H12B), C13(H13A,H13B), C15(H15A,H15B), C20(H20A,H20B),
  C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B), C27(H27A,H27B), C29(H29A,
 H29B), C31(H31A,H31B), C33(H33A,H33B)
4.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18)
4.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C16(H16A,H16B,H16C), C21(H21A,H21B,H21C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,
 H34B,H34C)
4.d Boron cage BH refined with riding coordinates:
 B5(H5), B6(H6), B7(H7), B8(H8), B9(H9), B10(H10)
;