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_7132122
_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         'C29 H45 Au B10 N2 O2'
_chemical_formula_sum            'C29 H45 Au B10 N2 O2'
_chemical_formula_weight         758.73
_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
_audit_creation_date             2022-12-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-07-11 deposited with the CCDC.	2023-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.835(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1127(4)
_cell_length_b                   26.6626(9)
_cell_length_c                   11.4450(4)
_cell_measurement_reflns_used    16340
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      30.9780
_cell_measurement_theta_min      1.9600
_cell_volume                     3350.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(11)
_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 0.832
_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    -26.00  24.00   0.50    3.00    --    5.00  57.00 -30.00  100
  2  \w     63.00  89.00   0.50    3.00    --    5.00  57.00 -30.00   52
  3  \w     23.00  49.00   0.50    3.00    --   -7.50  57.00  90.00   52
  4  \w     -7.00  20.00   0.50    3.00    --   -7.50 -57.00   0.00   54
  5  \w    -96.00  30.00   0.50    3.00    --   -7.50 -38.00  90.00  252
  6  \w    -96.00  76.00   0.50    3.00    --   -7.50  19.00  60.00  344
;
_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      0.0643550000
_diffrn_orient_matrix_UB_12      -0.0001719000
_diffrn_orient_matrix_UB_13      0.0155018000
_diffrn_orient_matrix_UB_21      0.0027602000
_diffrn_orient_matrix_UB_22      -0.0229527000
_diffrn_orient_matrix_UB_23      -0.0307871000
_diffrn_orient_matrix_UB_31      0.0054844000
_diffrn_orient_matrix_UB_32      0.0134184000
_diffrn_orient_matrix_UB_33      -0.0523838000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.832
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            44387
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.832
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.882
_diffrn_reflns_theta_min         1.527
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    4.421
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.64a (Rigaku Oxford Diffraction, 2022)
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    1.504
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.063
_refine_diff_density_min         -1.010
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         8795
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0159P)^2^+3.6635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0466
_refine_ls_wR_factor_ref         0.0487
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7478
_reflns_number_total             8795
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04091g2.cif
_cod_data_source_block           MesDACAuCarbiPr
_cod_database_code               7132122
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C30B2H10N2Au1O2
_shelx_estimated_absorpt_t_max   0.692
_shelx_estimated_absorpt_t_min   0.430
_diffrn_oxdiff_digest_frames
;
015e5b8cf06c861a4050dec483344fb6260002642cf
;
_diffrn_oxdiff_digest_hkl
;
0177eb10756571ca312e56c6c1dd1757661546
;
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C3(H3)
2.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C16(H16), C14(H14), C25(H25)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C28(H28A,H28B,H28C), C20(H20A,H20B,H20C), C11(H11A,H11B,
 H11C), C27(H27A,H27B,H27C), C4(H4A,H4B,H4C), C29(H29A,H29B,H29C), C19(H19A,
 H19B,H19C), C10(H10A,H10B,H10C), C5(H5A,H5B,H5C)
2.d Boron cage BH refined with riding coordinates:
 B3(H3A), B9(H9), B5(H5), B12(H12), B7(H7), B11(H11), B4(H4), B8(H8), B10(H10),
  B6(H6)
;
_shelx_res_checksum              12855
_shelx_hkl_checksum              90941
_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 1.298
_oxdiff_exptl_absorpt_empirical_full_min 0.839