Tethered N-heterocyclic carbene-carboranes: unique ligands that exhibit unprecedented and versatile coordination modes at rhodium
Jordan Holmes; Christopher M. Pask; Mark A. Fox; Charlotte E. Willans; Chem.Commun. 52 (2016) 6443–; doi:

data_7119095
_publ_section_title
;
 Tethered N-heterocyclic carbene-carboranes: unique ligands that exhibit
 unprecedented and versatile coordination modes at rhodium
;
_journal_name_full               Chem.Commun.
_journal_page_first              6443
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C27 H49 B9 N2 Rh2, 0.5(C4 H10 O)'
_chemical_formula_sum            'C29 H54 B9 N2 O0.5 Rh2'
_chemical_formula_weight         741.85
_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             2015-09-08
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-12-23 deposited with the CCDC.
2016-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                71.730(9)
_cell_angle_beta                 83.274(6)
_cell_angle_gamma                69.415(8)
_cell_formula_units_Z            2
_cell_length_a                   10.7898(6)
_cell_length_b                   11.4212(12)
_cell_length_c                   14.8764(14)
_cell_measurement_reflns_used    5549
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      30.3060
_cell_measurement_theta_min      3.4990
_cell_volume                     1629.6(3)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET) (compiled Jun 10 2013,11:58:50)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET) (compiled Jun 10 2013,11:58:50)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET) (compiled Jun 10 2013,11:58:50)'
_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      120.01(10)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega    8.00   33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884   37.0000   60.0000 25

  2 omega   31.00   56.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       13.1072   57.0000  150.0000 25

  3 omega  -10.00   17.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       13.1072   57.0000  150.0000 27

  4 omega  -12.00   82.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       13.1072   57.0000   30.0000 94

  5 omega  -29.00    0.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884  -64.0000  -95.6670 29

  6 omega  -79.00  -48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884  -64.0000  -95.6670 31

  7 omega  -34.00   54.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884   57.0000  -90.0000 88

  8 omega  -64.00    4.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884  -37.0000  120.0000 68

  9 omega  -70.00   10.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884  -61.0000   93.8040 80
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0285835000
_diffrn_orient_matrix_UB_12      0.0686064000
_diffrn_orient_matrix_UB_13      -0.0200385000
_diffrn_orient_matrix_UB_21      0.0078721000
_diffrn_orient_matrix_UB_22      -0.0082346000
_diffrn_orient_matrix_UB_23      -0.0458873000
_diffrn_orient_matrix_UB_31      -0.0636584000
_diffrn_orient_matrix_UB_32      -0.0062683000
_diffrn_orient_matrix_UB_33      0.0037527000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0627
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19367
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.20
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.039
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.731
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET) (compiled Jun 10 2013,11:58:50) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)'
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             762
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.546
_refine_diff_density_min         -1.401
_refine_diff_density_rms         0.135
_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     400
_refine_ls_number_reflns         8069
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0333P)^2^+6.6324P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1177
_reflns_number_gt                6104
_reflns_number_total             8069
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc01650b2.cif
_cod_data_source_block           Complex_4_dash
_cod_original_cell_volume        1629.6(2)
_cod_original_formula_sum        'C29 H54 B9 N2 O0.50 Rh2'
_cod_database_code               7119095
_chemical_oxdiff_formula         'C58 H108 B18 N4 O1 Rh4 '
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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
 C31-C28 = C30-C29
 1.5 with sigma of 0.02
 O1-C29 = O1-C28
 1.4 with sigma of 0.005
3. Rigid bond restraints
 C20, C21, C22, C23, C24, C25, C26, C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C20 \\sim C21 \\sim C22 \\sim C24 \\sim C25 \\sim C26 \\sim C27: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C21) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C26) \\sim Ueq,
Uanis(C25) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Others
 Fixed Sof: C9B(0.35) H9BA(0.35) H9BB(0.35) H9BC(0.35) C10B(0.35) H10A(0.35)
 H10B(0.35) H10C(0.35) C11B(0.35) H11A(0.35) H11B(0.35) H11C(0.35) C29(0.5)
 H29A(0.5) H29B(0.5) C9A(0.65) H9AA(0.65) H9AB(0.65) H9AC(0.65) C10A(0.65)
 H10D(0.65) H10E(0.65) H10F(0.65) C11A(0.65) H11D(0.65) H11E(0.65) H11F(0.65)
 C28(0.5) H28A(0.5) H28B(0.5) C30(0.5) H30A(0.5) H30B(0.5) H30C(0.5) C31(0.5)
 H31A(0.5) H31B(0.5) H31C(0.5)
6.a Ternary CH refined with riding coordinates:
 C12(H12A), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C24(H24), C25(H25)
6.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C13(H13A,H13B), C14(H14A,H14B), C17(H17A,H17B),
 C18(H18A,H18B), C22(H22A,H22B), C23(H23A,H23B), C26(H26A,H26B), C27(H27A,H27B),
  C29(H29A,H29B), C28(H28A,H28B)
6.c Me refined with riding coordinates:
 C9B(H9BA,H9BB,H9BC), C10B(H10A,H10B,H10C), C11B(H11A,H11B,H11C), C9A(H9AA,
 H9AB,H9AC), C10A(H10D,H10E,H10F), C11A(H11D,H11E,H11F), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C)
6.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6)
6.e Boron cage BH refined with riding coordinates:
 C1(H1), B4(H4), B8(H8), B7(H7), B6(H6A), B5(H5A), B9(H9), B12(H12), B11(H11),
 B10(H10)
;
_olex2_submission_special_instructions 'No special instructions were received'