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_7119097
_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         'C19 H37 B10 N2 Rh'
_chemical_formula_sum            'C19 H37 B10 N2 Rh'
_chemical_formula_weight         504.52
_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             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                 113.020(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2832(5)
_cell_length_b                   10.5283(2)
_cell_length_c                   14.1775(4)
_cell_measurement_reflns_used    8794
_cell_measurement_temperature    119.99(10)
_cell_measurement_theta_max      30.7310
_cell_measurement_theta_min      3.7320
_cell_volume                     2374.34(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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_environment      N~2~
_diffrn_ambient_temperature      119.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega    4.00   58.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       12.9509   57.0000   60.0000 54

  2 omega  -11.00   50.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       12.9509   57.0000    0.0000 61

  3 omega   12.00   80.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       12.9509   37.0000  -90.0000 68

  4 omega   13.00   38.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       12.9509  -57.0000  -60.0000 25

  5 omega  -41.00  -16.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       12.9509  -57.0000  -60.0000 25

  6 omega  -84.00  -39.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -13.7322  -37.0000   60.0000 45

  7 omega  -57.00  -32.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       12.9509  -37.0000  150.0000 25

  8 omega    8.00   33.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       12.9509  -37.0000  150.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0185580000
_diffrn_orient_matrix_UB_12      -0.0504983000
_diffrn_orient_matrix_UB_13      -0.0345939000
_diffrn_orient_matrix_UB_21      -0.0249001000
_diffrn_orient_matrix_UB_22      0.0442929000
_diffrn_orient_matrix_UB_23      -0.0371889000
_diffrn_orient_matrix_UB_31      0.0319898000
_diffrn_orient_matrix_UB_32      0.0051704000
_diffrn_orient_matrix_UB_33      -0.0193891000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0891
_diffrn_reflns_av_unetI/netI     0.0773
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20821
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.06
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.731
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_correction_T_min  0.754
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) 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) 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    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.295
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         5881
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0393P)^2^+0.9499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1155
_reflns_number_gt                4816
_reflns_number_total             5881
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc01650b2.cif
_cod_data_source_block           Complex-6
_cod_original_cell_volume        2374.33(10)
_cod_database_code               7119097
_chemical_oxdiff_formula         'C76 H148 B40 N8 Rh4 O1 '
_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.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C16(H16), C19(H19)
2.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)
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)
2.e Boron cage BH refined with riding coordinates:
 B3(H3), B4(H4), B5(H5A), B6(H6A), B7(H7), B8(H8), B9(H9), B10(H10), B11(H11),
 B12(H12A)
;
_olex2_submission_special_instructions 'No special instructions were received'