Highly phosphorescent Carbene-Metal-Carboranyl complexes of Copper(I) and Gold(I)
Powley, Samuel L.; Riley, Charlotte; Cho, Hwan-Hee; Phuoc, Nguyen Le; Greenham, N. C.; Linnolahti, Mikko; Romanov, Alexander S.; Chemical Communications  (2023) –; doi:10.1039/D3CC04091G

data_7132123
_publ_section_title
;
 Highly phosphorescent Carbene-Metal-Carboranyl complexes of Copper(I) and
 Gold(I)
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC04091G
_journal_year                    2023
_chemical_formula_moiety         'C32 H43 Au B10 N2 O2'
_chemical_formula_sum            'C32 H43 Au B10 N2 O2'
_chemical_formula_weight         792.75
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-06
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_audit_update_record
;
2023-07-11 deposited with the CCDC.	2023-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.8610(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.53700(10)
_cell_length_b                   18.0731(2)
_cell_length_c                   20.1419(2)
_cell_measurement_reflns_used    21026
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.2940
_cell_measurement_theta_min      3.2750
_cell_volume                     3815.70(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.80a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.80a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.80a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -47.00 -22.00   0.50    0.50    --    5.00 -54.00 -76.00   50
  2  \w      9.00  34.00   0.50    0.50    --    5.00  54.00  67.00   50
  3  \w    -73.00 -32.00   0.50    0.50    --  -44.40 -54.00 -76.00   82
  4  \w    -35.00  31.00   0.50    0.50    --  -44.40  54.00  67.00  132
  5  \w    -99.00 -74.00   0.50    0.50    --  -46.40 -54.00 -76.00   50
  6  \w    -42.00 -17.00   0.50    0.50    --  -46.40  54.00  67.00   50
  7  \w   -107.00 -18.00   0.50    1.15    -- -107.20  54.00  67.00  178
  8  \w   -161.00-118.00   0.50    1.15    -- -107.20 -54.00 -76.00   86
  9  \w    -48.00  30.00   0.50    0.50    --    5.00 -57.00 150.00  156
 10  \w     10.00  37.00   0.50    0.50    --    5.00  57.00-180.00   54
 11  \w    -28.00  -3.00   0.50    0.50    --  -44.40  57.00-180.00   50
 12  \w   -136.00 -13.00   0.50    0.50    --  -46.40 -57.00 150.00  246
 13  \w    -79.00  42.00   0.50    0.50    --  -46.40  57.00 120.00  242
 14  \w    -86.00  42.00   0.50    0.50    --  -46.40  76.00 -30.00  256
 15  \w    -99.00 -67.00   0.50    1.15    -- -107.20 -76.00-150.00   64
 16  \w   -197.00 -75.00   0.50    1.15    -- -107.20 -57.00 -30.00  244
 17  \w   -172.00-146.00   0.50    1.15    -- -107.20 -76.00-150.00   52
 18  \w   -177.00-150.00   0.50    1.15    -- -107.20 -38.00-150.00   54
 19  \w   -104.00 -71.00   0.50    1.15    -- -107.20 -76.00-180.00   66
 20  \w   -185.00-158.00   0.50    1.15    -- -107.20 -51.00 168.16   54
 21  \w   -116.00 -75.00   0.50    1.15    -- -107.20 -51.00 168.16   82
 22  \w   -196.00 -69.00   0.50    1.15    -- -107.20 -38.00-120.00  254
 23  \w   -137.00 -70.00   0.50    1.15    -- -107.20 -76.00  60.00  134
 24  \w   -132.00-107.00   0.50    1.15    -- -107.20 -57.00  60.00   50
 25  \w   -195.00-142.00   0.50    1.15    -- -107.20 -57.00  60.00  106
 26  \w   -193.00-159.00   0.50    1.15    -- -107.20 -76.00  60.00   68
 27  \w   -102.00 -74.00   0.50    1.15    -- -107.20 -76.00  30.00   56
 28  \w   -195.00-111.00   0.50    1.15    -- -107.20 -76.00  30.00  168
 29  \w   -166.00 -93.00   0.50    1.15    -- -107.20 -57.00 150.00  146
 30  \w    -96.00 -70.00   0.50    1.15    -- -107.20 -38.00-150.00   52
 31  \w   -197.00 -92.00   0.50    1.15    -- -107.20 -57.00   0.00  210
 32  \w   -194.00 -35.00   0.50    1.15    -- -107.20 -19.00  60.00  318
 33  \w   -185.00 -68.00   0.50    1.15    -- -107.20 -38.00-180.00  234
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0224118000
_diffrn_orient_matrix_UB_12      0.0559882000
_diffrn_orient_matrix_UB_13      0.0552457000
_diffrn_orient_matrix_UB_21      -0.1449145000
_diffrn_orient_matrix_UB_22      -0.0041828000
_diffrn_orient_matrix_UB_23      -0.0199935000
_diffrn_orient_matrix_UB_31      -0.0102156000
_diffrn_orient_matrix_UB_32      -0.0641752000
_diffrn_orient_matrix_UB_33      0.0495422000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            49649
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.852
_diffrn_reflns_theta_min         4.218
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    7.461
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81002
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.80a (Rigaku Oxford Diffraction, 2023)
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    1.380
_exptl_crystal_description       block
_exptl_crystal_F_000             1576
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.774
_refine_diff_density_min         -1.198
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         7884
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+5.2860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0675
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7195
_reflns_number_total             7884
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04091g2.cif
_cod_data_source_block           DAC_Mes_AuPhCarb
_cod_database_code               7132123
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H20N2Au1B10O2
_shelx_estimated_absorpt_t_max   0.444
_shelx_estimated_absorpt_t_min   0.317
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C13-C14 = C13A-C14A = C10-C12
 0.01 with sigma of 2.533
3. Uiso/Uaniso restraints and constraints
Uanis(C11A) = Uanis(C14A) = Uanis(C14) = Uanis(C13A) = Uanis(C13)
4. Others
 Fixed Sof: C13(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C14A(0.5) H14A(0.5)
 H14B(0.5) H14C(0.5) C14(0.5) H14D(0.5) H14E(0.5) H14F(0.5) C13A(0.5) H13D(0.5)
 H13E(0.5) H13F(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C4(H4), C8(H8), C7(H7), C28(H28), C17(H17), C19(H19), C5(H5), C26(H26)
5.b Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C21(H21A,H21B,H21C), C31(H31A,H31B,H31C), C30(H30A,H30B,
 H30C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C13(H13A,H13B,H13C),
 C14A(H14A,H14B,H14C), C14(H14D,H14E,H14F), C13A(H13D,H13E,H13F)
5.c Boron cage BH refined with riding coordinates:
 B3(H3), B11(H11), B10(H10), B7(H7A), B6(H6A), B12(H12), B9(H9), B5(H5A),
 B8(H8A), B4(H4A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              78578
_shelx_hkl_checksum              98339
_shelx_fab_checksum              47676
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.222
_oxdiff_exptl_absorpt_empirical_full_min 0.869