Synthesis and full characterization of an iridium B-H activation intermediate of the monocarba-closo-dodecaborate anion.
Shen, Yunjun; Pan, Yani; Liu, Jiyong; Sattasathuchana, Tosaporn; Baldridge, Kim K.; Duttwyler, Simon; Chemical communications (Cambridge, England) 53 (2016) 176–179; doi:10.1039/c6cc08121e

data_7119607
_publ_section_title
;
 Synthesis and full characterization of an iridium B-H activation
 intermediate of the monocarba-closo-dodecaborate anion.
;
_journal_issue                   1
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              176
_journal_page_last               179
_journal_paper_doi               10.1039/c6cc08121e
_journal_volume                  53
_journal_year                    2016
_chemical_formula_moiety         'C21 H35 B11 Ir N2 O3 S, C8 H20 N'
_chemical_formula_sum            'C29 H55 B11 Ir N3 O3 S'
_chemical_formula_weight         836.93
_chemical_name_systematic
;
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-12-25
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2016-10-06 deposited with the CCDC.
2016-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 107.086(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.5995(15)
_cell_length_b                   11.8627(4)
_cell_length_c                   22.3097(8)
_cell_measurement_reflns_used    5222
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1417
_cell_measurement_theta_min      2.8598
_cell_volume                     7993.8(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
;
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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0081277000
_diffrn_orient_matrix_UB_12      0.0239508000
_diffrn_orient_matrix_UB_13      0.0235920000
_diffrn_orient_matrix_UB_21      0.0135752000
_diffrn_orient_matrix_UB_22      0.0480424000
_diffrn_orient_matrix_UB_23      0.0011154000
_diffrn_orient_matrix_UB_31      -0.0173423000
_diffrn_orient_matrix_UB_32      0.0263688000
_diffrn_orient_matrix_UB_33      -0.0234163000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            16133
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.01
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.426
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49834
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.256
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         7312
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0592P)^2^+12.1276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1095
_reflns_number_gt                5890
_reflns_number_total             7312
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc08121e2.cif
_cod_data_source_block           141225_yjs_0094
_cod_database_code               7119607
_chemical_oxdiff_formula         c21h23n1o4s1Ir1
_reflns_odcompleteness_completeness 99.63
_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
C10 \\sim C14 \\sim C12 \\sim C11 \\sim C13 \\sim C15 \\sim C16 \\sim C17 \\sim
C19 \\sim C18: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02
3.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C24(H24A,H24B), C26(H26A,H26B), C28(H28A,H28B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4A), C5(H5A), C7(H7), C8(H8)
3.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C23(H23A,
 H23B,H23C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C)
3.d Boron cage BH refined with riding coordinates:
 B1(H1), B3(H3), B4(H4), B5(H5), B6(H6), B7(H7A), B8(H8A), B9(H9), B10(H10),
 B11(H11)
;