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_7119093
_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         'C29 H52 B9 N3 Rh2, C2 H3 N'
_chemical_formula_sum            'C31 H55 B9 N4 Rh2'
_chemical_formula_weight         786.90
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.9249(5)
_cell_length_b                   23.7834(11)
_cell_length_c                   25.2349(11)
_cell_measurement_reflns_used    7857
_cell_measurement_temperature    120.00(11)
_cell_measurement_theta_max      30.5930
_cell_measurement_theta_min      3.6920
_cell_volume                     7157.0(5)
_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      120.00(11)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   17.00   53.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7322   37.0000  150.0000 36

  2 omega  -41.00    8.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7322   19.0000   30.0000 49

  3 omega  -15.00   20.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7322  -19.0000  120.0000 35

  4 omega  -83.00  -20.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7322  -37.0000  -30.0000 63

  5 omega  -34.00   14.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7322   37.0000  150.0000 48
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0084254000
_diffrn_orient_matrix_UB_12      0.0207783000
_diffrn_orient_matrix_UB_13      -0.0197725000
_diffrn_orient_matrix_UB_21      -0.0548604000
_diffrn_orient_matrix_UB_22      0.0104672000
_diffrn_orient_matrix_UB_23      0.0045945000
_diffrn_orient_matrix_UB_31      0.0213550000
_diffrn_orient_matrix_UB_32      0.0186764000
_diffrn_orient_matrix_UB_33      0.0194339000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0852
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            43820
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.23
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.951
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.897
_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    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.149
_refine_diff_density_min         -1.547
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         8855
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0218P)^2^+14.2129P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0997
_reflns_number_gt                6795
_reflns_number_total             8855
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc01650b2.cif
_cod_data_source_block           Complex-3
_cod_original_cell_volume        7157.0(6)
_cod_database_code               7119093
_chemical_oxdiff_formula         'C248 H440 B72 N32 Rh16 '
_reflns_odcompleteness_completeness 99.72
_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.a Ternary CH refined with riding coordinates:
 C12(H12A), C13(H13), C16(H16), C17(H17), C22(H22), C25(H25), C26(H26), C29(H29)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C14(H14A,H14B), C15(H15A,H15B), C18(H18A,H18B),
 C19(H19A,H19B), C23(H23A,H23B), C24(H24A,H24B), C27(H27A,H27B), C28(H28A,H28B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6)
2.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C21(H21A,H21B,
 H21C), C32(H32A,H32B,H32C)
2.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'