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_7119091
_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         'C11 H27 B10 N2, 0.5(C2 H3 N), Br'
_chemical_formula_sum            'C12 H28.5 B10 Br N2.5'
_chemical_formula_weight         395.88
_chemical_name_systematic        'Compound 1'
_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                 92.279(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.6257(3)
_cell_length_b                   25.7293(10)
_cell_length_c                   10.2076(6)
_cell_measurement_reflns_used    4486
_cell_measurement_temperature    119.99(14)
_cell_measurement_theta_max      30.8090
_cell_measurement_theta_min      4.1360
_cell_volume                     2001.19(16)
_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 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.99(14)
_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   24.00   59.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509   57.0000  -30.0000 35

  2 omega   40.00   67.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509   37.0000   30.0000 27

  3 omega  -11.00   73.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509   57.0000  150.0000 84

  4 omega  -19.00   33.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509  -37.0000 -120.0000 52

  5 omega  -43.00    2.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509  -37.0000   30.0000 45
;
_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      -0.0132653000
_diffrn_orient_matrix_UB_12      -0.0219840000
_diffrn_orient_matrix_UB_13      0.0403530000
_diffrn_orient_matrix_UB_21      0.0360326000
_diffrn_orient_matrix_UB_22      0.0137956000
_diffrn_orient_matrix_UB_23      0.0548849000
_diffrn_orient_matrix_UB_31      -0.0848085000
_diffrn_orient_matrix_UB_32      0.0092942000
_diffrn_orient_matrix_UB_33      0.0139508000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13430
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.11
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.053
_exptl_absorpt_correction_T_max  0.848
_exptl_absorpt_correction_T_min  0.586
_exptl_absorpt_correction_type   gaussian
_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)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         4963
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0349P)^2^+1.9377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0969
_reflns_number_gt                4047
_reflns_number_total             4963
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc01650b2.cif
_cod_data_source_block           Imidazolium-Bromide-Salt-1
_cod_original_cell_volume        2001.19(15)
_cod_original_formula_sum        'C12 H28.50 B10 Br N2.50'
_cod_database_code               7119091
_chemical_oxdiff_formula         'C48 H114 B40 Br4 N10'
_reflns_odcompleteness_completeness 99.82
_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
 N3-C12
 1.14 with sigma of 0.01
 C13-C12
 1.45 with sigma of 0.02
3. Others
 Fixed Sof: C13(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C12(0.5) N3(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B)
4.b Me refined with riding coordinates:
 C13(H13A,H13B,H13C)
4.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7)
4.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
4.e Boron cage BH refined with riding coordinates:
 C1(H1), B3(H3), B4(H4), B5(H5A), B6(H6A), B7(H7A), B8(H8), B9(H9), B10(H10),
 B11(H11), B12(H12)
;
_olex2_date_sample_data_collection 2015-04-14
_olex2_submission_special_instructions 'No special instructions were received'