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_7132124
_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         'C35 H57 Au B10 N2 O2'
_chemical_formula_sum            'C35 H57 Au B10 N2 O2'
_chemical_formula_weight         842.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-06
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-07-11 deposited with the CCDC.	2023-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.0324(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.48602(12)
_cell_length_b                   19.7064(2)
_cell_length_c                   17.35568(19)
_cell_measurement_reflns_used    16155
_cell_measurement_temperature    100.00(13)
_cell_measurement_theta_max      75.6210
_cell_measurement_theta_min      3.3860
_cell_volume                     3922.92(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (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(13)
_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 0.973
_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      8.00  33.00   0.50    0.50    --    5.00  66.00-106.00   50
  2  \w    -46.00 -21.00   0.50    0.50    --    5.00 -66.00 118.00   50
  3  \w   -120.00 -20.00   0.50    0.50    --  -44.40 -66.00 118.00  200
  4  \w    -68.00  12.00   0.50    0.50    --  -46.40  66.00-106.00  160
  5  \w   -152.00-109.00   0.50    0.50    -- -107.20 -66.00 118.00   86
  6  \w   -135.00 -18.00   0.50    0.50    -- -107.20  66.00-106.00  234
  7  \w   -101.00 -23.00   0.50    0.50    --  -44.40 -57.00   0.00  156
  8  \w   -197.00-156.00   0.50    0.50    -- -107.20 -57.00  30.00   82
  9  \w   -106.00 -30.00   0.50    0.50    -- -107.20  76.00  30.00  152
 10  \w   -197.00 -74.00   0.50    0.50    -- -107.20 -57.00  90.00  246
 11  \w   -197.00 -99.00   0.50    0.50    -- -107.20 -57.00-180.00  196
 12  \w   -140.00 -84.00   0.50    0.50    -- -107.20 -57.00  30.00  112
 13  \w   -196.00-112.00   0.50    0.50    -- -107.20 -57.00-150.00  168
;
_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      -0.0140022000
_diffrn_orient_matrix_UB_12      -0.0587854000
_diffrn_orient_matrix_UB_13      -0.0582126000
_diffrn_orient_matrix_UB_21      0.1335494000
_diffrn_orient_matrix_UB_22      -0.0060316000
_diffrn_orient_matrix_UB_23      -0.0016418000
_diffrn_orient_matrix_UB_31      0.0005021000
_diffrn_orient_matrix_UB_32      -0.0511417000
_diffrn_orient_matrix_UB_33      0.0672180000
_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  0.0214
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23741
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.958
_diffrn_reflns_theta_min         3.396
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    7.286
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
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    1.427
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.000169(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         7971
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0230
_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^)+(0.0317P)^2^+4.1673P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0635
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7566
_reflns_number_total             7971
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04091g2.cif
_cod_data_source_block           DippDACAuCarb
_cod_original_cell_volume        3922.93(7)
_cod_database_code               7132124
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H20B10N2O2Au1
_shelx_estimated_absorpt_t_max   0.669
_shelx_estimated_absorpt_t_min   0.408
_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.a Ternary CH refined with riding coordinates:
 C18(H18), C3(H3), C21(H21), C33(H33), C30(H30)
2.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C14(H14), C15(H15), C27(H27), C28(H28), C16(H16)
2.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C5(H5A,H5B,H5C), C11(H11A,H11B,H11C), C20(H20A,H20B,
 H20C), C4(H4A,H4B,H4C), C10(H10A,H10B,H10C), C22(H22A,H22B,H22C), C34(H34A,
 H34B,H34C), C23(H23A,H23B,H23C), C35(H35A,H35B,H35C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C)
2.d Boron cage BH refined with riding coordinates:
 B11(H11), B6(H6), B8(H8), B10(H10), B7(H7), B4(H4), B12(H12), B9(H9), B5(H5),
 B3(H3A)
;
_shelx_res_checksum              26052
_shelx_hkl_checksum              85308
_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 1.406
_oxdiff_exptl_absorpt_empirical_full_min 0.784