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_7132125
_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 B10 Cu N2 O2, C3 H7'
_chemical_formula_sum            'C35 H50 B10 Cu N2 O2'
_chemical_formula_weight         702.41
_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   mixed
_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                 96.5490(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.63269(10)
_cell_length_b                   18.25848(15)
_cell_length_c                   19.63777(18)
_cell_measurement_reflns_used    18529
_cell_measurement_temperature    99.99(17)
_cell_measurement_theta_max      75.9130
_cell_measurement_theta_min      3.2760
_cell_volume                     3787.54(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (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      99.99(17)
_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 0.987
_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    -46.00  77.00   0.50    0.71    --   43.87  60.00-120.00  246
  2  \w     88.00 132.00   0.50    0.71    --   43.87  60.00-120.00   88
  3  \w     87.00 136.00   0.50    0.71    --   46.33  40.00 -90.00   98
  4  \w    -42.00 123.00   0.50    0.71    --   46.33   0.00 -30.00  330
  5  \w     63.00 105.00   0.50    0.71    --   46.33   0.00-180.00   84
  6  \w      9.00  58.00   0.50    0.71    --   46.33  10.00  90.00   98
  7  \w    -39.00 -13.00   0.50    0.71    --   46.33  10.00  90.00   52
  8  \w     89.00 116.00   0.50    0.71    --   46.33  10.00  90.00   54
  9  \w     19.00  44.00   0.50    2.85    --  108.20  58.00-133.75   50
 10  \w     34.00  60.00   0.50    2.85    --  108.20  40.00   0.00   52
 11  \w     21.00  70.00   0.50    2.85    --  108.20  44.00-124.06   98
 12  \w     83.00 191.00   0.50    2.85    --  108.20  40.00   0.00  216
 13  \w    115.00 140.00   0.50    2.85    --  108.20  50.00 -30.00   50
 14  \w    147.00 175.00   0.50    2.85    --  108.20  50.00 -30.00   56
 15  \w     96.00 198.00   0.50    2.85    --  108.20  59.00-121.25  204
 16  \w     69.00 189.00   0.50    2.85    --  108.20  20.00   0.00  240
 17  \w     19.00  44.00   0.50    2.85    --  108.20  50.00-134.50   50
 18  \w     19.00  81.00   0.50    2.85    --  108.20  50.00  30.00  124
 19  \w    129.00 170.00   0.50    2.85    --  108.20  50.00  30.00   82
 20  \w     19.00  64.00   0.50    2.85    --  108.20  20.00   0.00   90
 21  \w     19.00  53.00   0.50    2.85    --  108.20  40.00-150.00   68
 22  \w     63.00 198.00   0.50    2.85    --  108.20  20.00-120.00  270
 23  \w    139.00 192.00   0.50    2.85    --  108.20   0.00-150.00  106
 24  \w     86.00 144.00   0.50    2.85    --  108.20  59.00-172.05  116
 25  \w     22.00  48.00   0.50    2.85    --  108.20  50.00   0.00   52
 26  \w    154.00 179.00   0.50    2.85    --  108.20  50.00   0.00   50
 27  \w     19.00  44.00   0.50    2.85    --  108.20  47.00-134.51   50
 28  \w     21.00 102.00   0.50    2.85    --  108.20  50.00-120.00  162
 29  \w    142.00 175.00   0.50    2.85    --  108.20  50.00-120.00   66
 30  \w     19.00  44.00   0.50    2.85    --  108.20  56.00-153.70   50
 31  \w     19.00  44.00   0.50    2.85    --  108.20  59.00-121.25   50
 32  \w     19.00  44.00   0.50    2.85    --  108.20  50.00-150.00   50
 33  \w     21.00 197.00   0.50    2.85    --  108.20  38.00-144.78  352
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0507072000
_diffrn_orient_matrix_UB_12      0.0734468000
_diffrn_orient_matrix_UB_13      0.0304971000
_diffrn_orient_matrix_UB_21      0.0165723000
_diffrn_orient_matrix_UB_22      0.0279358000
_diffrn_orient_matrix_UB_23      -0.0724695000
_diffrn_orient_matrix_UB_31      -0.1356956000
_diffrn_orient_matrix_UB_32      0.0308411000
_diffrn_orient_matrix_UB_33      -0.0072194000
_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  0.0398
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            47417
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.089
_diffrn_reflns_theta_min         3.315
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    1.058
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.81a (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    1.232
_exptl_crystal_description       block
_exptl_crystal_F_000             1476
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         7822
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+2.4049P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1063
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6846
_reflns_number_total             7822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04091g2.cif
_cod_data_source_block           DAC_Mes_Cu_CarbPh
_cod_original_cell_volume        3787.53(6)
_cod_database_code               7132125
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C28H20N2O2B10Cu1
_shelx_estimated_absorpt_t_max   0.857
_shelx_estimated_absorpt_t_min   0.824
_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 Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B)
2.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C17(H17), C4(H4), C28(H28), C5(H5), C26(H26), C8(H8), C6(H6), C7(H7)
2.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C21(H21A,H21B,H21C), C30(H30A,H30B,H30C), C23(H23A,H23B,
 H23C), C33(H33A,H33B,H33C), C22(H22A,H22B,H22C), C14(H14A,H14B,H14C), C13(H13A,
 H13B,H13C), C31(H31A,H31B,H31C)
2.d Boron cage BH refined with riding coordinates:
 B3(H3), B7(H7A), B8(H8A), B6(H6A), B5(H5A), B4(H4A), B11(H11), B10(H10),
 B12(H12), B9(H9)
;
_shelx_res_checksum              58481
_shelx_hkl_checksum              90743
_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 1.817
_oxdiff_exptl_absorpt_empirical_full_min 0.709