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_7132126
_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 B10 Cu N2 O2'
_chemical_formula_sum            'C29 H45 B10 Cu N2 O2'
_chemical_formula_weight         625.31
_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                 97.260(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9247(2)
_cell_length_b                   26.7491(4)
_cell_length_c                   11.4847(2)
_cell_measurement_reflns_used    11744
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.8290
_cell_measurement_theta_min      3.5580
_cell_volume                     3329.22(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1428
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.875
_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    -91.00 -63.00   1.00   11.00    --  -18.62-178.00-120.00   28
  2  \w    -75.00  -9.00   1.00   11.00    --  -18.62 -37.00   0.00   66
  3  \w    -11.00  20.00   1.00   11.00    --   20.34  77.00 -30.00   31
  4  \w    -47.00  77.00   1.00   11.00    --   20.34   0.00-120.00  124
  5  \w     -4.00  42.00   1.00   11.00    --   20.34  77.00   0.00   46
  6  \w     -7.00  40.00   1.00   11.00    --   20.34  77.00-120.00   47
  7  \w    -11.00  40.00   1.00   11.00    --   20.34  77.00 120.00   51
  8  \w     12.00  42.00   1.00   11.00    --   20.34 -57.00  60.00   30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0253876000
_diffrn_orient_matrix_UB_12      0.0244464000
_diffrn_orient_matrix_UB_13      0.0040326000
_diffrn_orient_matrix_UB_21      -0.0504130000
_diffrn_orient_matrix_UB_22      0.0088433000
_diffrn_orient_matrix_UB_23      -0.0395999000
_diffrn_orient_matrix_UB_31      -0.0331224000
_diffrn_orient_matrix_UB_32      0.0052553000
_diffrn_orient_matrix_UB_33      0.0478602000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.875
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27413
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.875
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.091
_diffrn_reflns_theta_min         3.533
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
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    1.248
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         7806
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0380P)^2^+2.3366P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0982
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6403
_reflns_number_total             7806
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04091g2.cif
_cod_data_source_block           MesDACCuCarbiPr
_cod_database_code               7132126
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H20N2B10Cu1O2
_shelx_estimated_absorpt_t_max   0.858
_shelx_estimated_absorpt_t_min   0.776
_diffrn_oxdiff_digest_frames
;
0123de8ab1bcb627e81def561992c3a2b100028f513
;
_diffrn_oxdiff_digest_hkl
;
011bdf9832ced2b4cb0ca4d47cc335608f29f2
;
_reflns_odcompleteness_completeness 99.73
_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:
 C14(H14), C26(H26), C16(H16), C23(H23)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C30(H30A,H30B,H30C), C28(H28A,H28B,H28C), C4(H4A,H4B,
 H4C), C29(H29A,H29B,H29C), C18(H18A,H18B,H18C), C10(H10A,H10B,H10C), C19(H19A,
 H19B,H19C), C11(H11A,H11B,H11C), C5(H5A,H5B,H5C)
2.d Boron cage BH refined with riding coordinates:
 B6(H6), B11(H11), B12(H12), B7(H7), B9(H9), B10(H10), B5(H5), B8(H8), B3(H3A),
  B4(H4)
;
_shelx_res_checksum              47303
_shelx_hkl_checksum              7910
_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 1.370
_oxdiff_exptl_absorpt_empirical_full_min 0.800