Light emission mechanism in dimers of carbene-metal-amide complexes.
Ruduss, Armands; Belyakov, Sergey; Stucere, Kitija A.; Vembris, Aivars; Traskovskis, Kaspars; Physical chemistry chemical physics : PCCP 25 (2023) 3220–3231; doi:10.1039/d2cp05237g

data_7246057
_publ_section_title
;
 Light emission mechanism in dimers of carbene-metal-amide complexes.
;
_journal_issue                   4
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              3220
_journal_page_last               3231
_journal_paper_doi               10.1039/d2cp05237g
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         '3(C29 H31 Cu N2 O2 S2), C12 H9 N O2 S'
_chemical_formula_sum            'C99 H102 Cu3 N7 O8 S7'
_chemical_formula_weight         1933.06
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     heavy
_audit_creation_date             2022-02-24
_audit_creation_method
;
Olex2 1.2-ac4
(compiled 2018.05.17 svn.r3504 for Rigaku Oxford Diffraction, GUI svn.r5492)
;
_audit_update_record
;
2022-09-25 deposited with the CCDC.	2022-12-27 downloaded from the CCDC.
;
_cell_angle_alpha                94.4120(10)
_cell_angle_beta                 100.8830(10)
_cell_angle_gamma                110.8080(10)
_cell_formula_units_Z            2
_cell_length_a                   12.21430(10)
_cell_length_b                   14.32990(10)
_cell_length_c                   28.98270(10)
_cell_measurement_reflns_used    66945
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      80.1130
_cell_measurement_theta_min      3.2140
_cell_volume                     4599.03(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9807
_diffrn_measured_fraction_theta_max 0.9807
_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    -79.00  21.00   0.50    0.26    --  -49.73  98.00  74.00  200
  2  \w     12.00  76.00   0.50    0.26    --   49.73 -98.00 -32.00  128
  3  \w   -148.00-123.00   0.50    1.05    --  -90.00 -98.00 -32.00   50
  4  \w    -73.00 -48.00   0.50    1.05    --  -90.00  98.00  74.00   50
  5  \w     60.00 105.00   0.50    1.05    --  111.50 -98.00 -32.00   90
  6  \w    106.00 145.00   0.50    1.05    --  111.50  98.00  74.00   78
  7  \w   -119.00 -88.00   0.50    0.26    --  -49.73 -77.00 120.00   62
  8  \w   -122.00 -90.00   0.50    0.26    --  -49.73 -77.00  90.00   64
  9  \w   -118.00 -93.00   0.50    0.26    --  -49.73 -77.00  60.00   50
 10  \w    -43.00  24.00   0.50    0.26    --  -49.73  19.00   0.00  134
 11  \w    -24.00  13.00   0.50    0.26    --  -49.73  57.00  30.00   74
 12  \w   -121.00 -90.00   0.50    0.26    --  -49.73 -77.00  30.00   62
 13  \w    -61.00 -33.00   0.50    0.26    --  -49.73  57.00  30.00   56
 14  \w     -4.00  43.00   0.50    0.26    --   49.73 -38.00  30.00   94
 15  \w    -44.00 -19.00   0.50    1.05    --  -90.00  30.00-120.00   50
 16  \w   -153.00-111.00   0.50    1.05    --  -90.00 -77.00  60.00   84
 17  \w    -46.00 -20.00   0.50    1.05    --  -90.00  15.00 -90.00   52
 18  \w    -44.00 -19.00   0.50    1.05    --  -90.00  30.00-180.00   50
 19  \w     98.00 136.00   0.50    1.05    --  111.50 -85.00 152.40   76
 20  \w     47.00  73.00   0.50    1.05    --  111.50 -85.00 152.40   52
 21  \w     41.00  66.00   0.50    1.05    --  111.50 -77.00-180.00   50
 22  \w     99.00 125.00   0.50    1.05    --  111.50-144.00 105.36   52
 23  \w     63.00  89.00   0.50    1.05    --  111.50-144.00 105.36   52
 24  \w     41.00  66.00   0.50    1.05    --  111.50 -61.00   0.00   50
 25  \w     81.00 106.00   0.50    1.05    --  111.50 -97.00 149.25   50
 26  \w    109.00 178.00   0.50    1.05    --  111.50  30.00  30.00  138
 27  \w     43.00  92.00   0.50    1.05    --  111.50 -94.00  90.00   98
 28  \w    104.00 178.00   0.50    1.05    --  111.50  30.00-120.00  148
 29  \w     41.00  67.00   0.50    1.05    --  111.50 -61.00-180.00   52
 30  \w     47.00 102.00   0.50    1.05    --  111.50-100.00 -55.82  110
 31  \w     41.00  67.00   0.50    1.05    --  111.50 -94.00  60.00   52
 32  \w     41.00 107.00   0.50    1.05    --  111.50-108.00 120.29  132
 33  \w    118.00 177.00   0.50    1.05    --  111.50  45.00  60.00  118
 34  \w     44.00  74.00   0.50    1.05    --  111.50 -77.00-150.00   60
 35  \w     41.00  90.00   0.50    1.05    --  111.50 -77.00  30.00   98
 36  \w    102.00 175.00   0.50    1.05    --  111.50  45.00 120.00  146
 37  \w     72.00 106.00   0.50    1.05    --  111.50-100.00   2.51   68
 38  \w     43.00  68.00   0.50    1.05    --  111.50-100.00   2.51   50
 39  \w     42.00 107.00   0.50    1.05    --  111.50-103.00 -66.66  130
 40  \w     41.00  66.00   0.50    1.05    --  111.50 -61.00-120.00   50
 41  \w     41.00  84.00   0.50    1.05    --  111.50 -94.00-150.00   86
 42  \w    105.00 176.00   0.50    1.05    --  111.50  15.00 -30.00  142
 43  \w     43.00  68.00   0.50    1.05    --  111.50 -61.00  30.00   50
 44  \w     41.00  66.00   0.50    1.05    --  111.50 -61.00 -60.00   50
 45  \w    105.00 163.00   0.50    1.05    --  111.50  30.00 -90.00  116
 46  \w     71.00 106.00   0.50    1.05    --  111.50-102.00  40.76   70
 47  \w     61.00 116.00   0.50    1.05    --  111.50-133.00 133.43  110
 48  \w     46.00  71.00   0.50    1.05    --  111.50 -77.00-120.00   50
 49  \w     59.00 105.00   0.50    1.05    --  111.50 -98.00 173.09   92
 50  \w    119.00 171.00   0.50    1.05    --  111.50  15.00-150.00  104
 51  \w     61.00 101.00   0.50    1.05    --  111.50 -94.00 120.00   80
 52  \w     45.00  72.00   0.50    1.05    --  111.50-115.00  -0.43   54
 53  \w     75.00 109.00   0.50    1.05    --  111.50-115.00  -0.43   68
 54  \w    109.00 135.00   0.50    1.05    --  111.50  30.00  90.00   52
 55  \w    144.00 170.00   0.50    1.05    --  111.50  30.00  90.00   52
 56  \w     44.00  78.00   0.50    1.05    --  111.50 -94.00   0.00   68
 57  \w    130.00 156.00   0.50    1.05    --  111.50 125.00   0.00   52
 58  \w     74.00  99.00   0.50    1.05    --  111.50 -94.00  60.00   50
 59  \w     41.00  66.00   0.50    1.05    --  111.50 -77.00 -60.00   50
 60  \w     48.00  73.00   0.50    1.05    --  111.50 -77.00  60.00   50
 61  \w    104.00 139.00   0.50    1.05    --  111.50  45.00   0.00   70
 62  \w     43.00  70.00   0.50    1.05    --  111.50 -94.00-180.00   54
 63  \w     52.00  77.00   0.50    1.05    --  111.50 -94.00 -90.00   50
 64  \w     82.00 107.00   0.50    1.05    --  111.50-102.00 129.26   50
 65  \w     42.00  93.00   0.50    1.05    --  111.50-125.00  60.00  102
 66  \w    123.00 149.00   0.50    1.05    --  111.50  15.00-120.00   52
 67  \w     73.00  98.00   0.50    1.05    --  111.50 -94.00-120.00   50
 68  \w     43.00  68.00   0.50    1.05    --  111.50-125.00-180.00   50
 69  \w     63.00 111.00   0.50    1.05    --  111.50-125.00 -90.00   96
 70  \w     86.00 111.00   0.50    1.05    --  111.50-125.00-120.00   50
 71  \w    106.00 168.00   0.50    1.05    --  111.50  15.00-180.00  124
 72  \w     43.00  71.00   0.50    1.05    --  111.50 -97.00 149.25   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku, XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0499301000
_diffrn_orient_matrix_UB_12      0.0703921000
_diffrn_orient_matrix_UB_13      0.0483137000
_diffrn_orient_matrix_UB_21      0.0704418000
_diffrn_orient_matrix_UB_22      -0.0651180000
_diffrn_orient_matrix_UB_23      0.0185625000
_diffrn_orient_matrix_UB_31      0.1085592000
_diffrn_orient_matrix_UB_32      0.0660691000
_diffrn_orient_matrix_UB_33      -0.0180270000
_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  0.0319
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            92885
_diffrn_reflns_theta_full        80.5287
_diffrn_reflns_theta_max         80.53
_diffrn_reflns_theta_min         3.14
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.775
_exptl_absorpt_correction_T_max  0.87431
_exptl_absorpt_correction_T_min  0.76053
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.3958
_exptl_crystal_description       'Block '
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.3618
_refine_diff_density_min         -0.4962
_refine_diff_density_rms         0.0567
_refine_ls_d_res_high            0.7816
_refine_ls_d_res_low             14.0545
_refine_ls_goodness_of_fit_ref   1.0354
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    166
_refine_ls_number_parameters     1139
_refine_ls_number_reflns         19798
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0354
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.0014
_refine_ls_shift/su_mean         0.0003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+2.1780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0916
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              18
_reflns_limit_k_min              -18
_reflns_limit_l_max              37
_reflns_limit_l_min              0
_reflns_number_gt                18782
_reflns_number_total             19798
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2cp05237g2.cif
_cod_data_source_block           PK14
_cod_depositor_comments
'Adding full bibliography for 7246057--7246058.cif.'
_cod_database_code               7246057
_chemical_oxdiff_formula         'C198 H204 Cu6 N14 O16 S14 '
_chemical_oxdiff_usercomment     'from Kaspars'
_diffrn_oxdiff_digest_frames
;
010f8d4af4756da0a76a5595819ed0993a000406bc7
;
_diffrn_oxdiff_digest_hkl
;
01a21f8abd0335e5413373a08a1018a86117b6
;
_reflns_odcompleteness_completeness 99.24
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C25(H25), C55(H55), C82(H82), C52(H52), C22(H22), C85(H85)
2.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C39(H39), C50(H50), C18(H18), C19(H19), C78(H78), C99(H99),
 C66(H66), C1(H1), C38(H38), C9(H9), C69(H69), C98(H98), C94(H94), C49(H49),
 C64(H64), C67(H67), C68(H68), C48(H48), C96(H96), C31(H31), C80(H80), C61(H61),
  C2(H2), C3(H3), C97(H97), C6(H6), C91(H91), C37(H37), C62(H62), C79(H79),
 C63(H63), C34(H34), C4(H4), C5(H5), C8(H8), C32(H32), C92(H92), C33(H33),
 C93(H93), C7(H7)
2.c Idealised Me refined as rotating group:
 C28(H28a,H28b,H28c), C58(H58a,H58b,H58c), C88(H88a,H88b,H88c), C59(H59a,H59b,
 H59c), C26(H26a,H26b,H26c), C89(H89a,H89b,H89c), C29(H29a,H29b,H29c), C23(H23a,
 H23b,H23c), C56(H56a,H56b,H56c), C54(H54a,H54b,H54c), C84(H84a,H84b,H84c),
 C83(H83a,H83b,H83c), C86(H86a,H86b,H86c), C57(H57a,H57b,H57c), C87(H87a,H87b,
 H87c), C53(H53a,H53b,H53c), C27(H27a,H27b,H27c), C24(H24a,H24b,H24c)
;
_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 1.470
_oxdiff_exptl_absorpt_empirical_full_min 0.684