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_7246058
_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         '4(C29 H31 Cu N2 O2 S2), C5 H10'
_chemical_formula_sum            'C121 H134 Cu4 N8 O8 S8'
_chemical_formula_weight         2338.99
_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
_audit_creation_date             2022-03-01
_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                90
_cell_angle_beta                 116.810(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.1244(3)
_cell_length_b                   35.6810(5)
_cell_length_c                   14.4150(3)
_cell_measurement_reflns_used    20984
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      79.9920
_cell_measurement_theta_min      3.6250
_cell_volume                     6024.8(2)
_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  'ShelXL (Sheldrick, 2015)'
_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 0.98
_diffrn_measured_fraction_theta_max 0.914
_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    -72.00 -20.00   0.50    2.00    --  -49.98  91.00  90.00  104
  2  \w    -46.00 -21.00   0.50    7.00    --  -90.00  33.00 -86.00   50
  3  \w     41.00  67.00   0.50    7.00    --  111.50-119.00-101.00   52
  4  \w    131.00 175.00   0.50    7.00    --  111.50  91.00  90.00   88
  5  \w    110.00 174.00   0.50    7.00    --  111.50  33.00 -86.00  128
  6  \w     82.00 108.00   0.50    7.00    --  111.50-119.00-101.00   52
  7  \w   -122.00 -88.00   0.50    2.00    --  -49.98 -77.00   0.00   68
  8  \w   -121.00 -94.00   0.50    2.00    --  -49.98 -77.00  60.00   54
  9  \w   -109.00 -83.00   0.50    2.00    --  -49.98-125.00-120.00   52
 10  \w     90.00 120.00   0.50    2.00    --   49.98  77.00 120.00   60
 11  \w     88.00 122.00   0.50    2.00    --   49.98  77.00 -30.00   68
 12  \w    -44.00 -19.00   0.50    7.00    --  -90.00  30.00 -60.00   50
 13  \w     42.00  68.00   0.50    7.00    --  111.50 -61.00 -30.00   52
 14  \w    110.00 141.00   0.50    7.00    --  111.50  30.00   0.00   62
 15  \w     41.00  66.00   0.50    7.00    --  111.50 -61.00  30.00   50
 16  \w     50.00  88.00   0.50    7.00    --  111.50 -77.00   0.00   76
 17  \w     45.00  76.00   0.50    7.00    --  111.50 -77.00  60.00   62
 18  \w    149.00 176.00   0.50    7.00    --  111.50  30.00   0.00   54
 19  \w     41.00  66.00   0.50    7.00    --  111.50 -61.00-150.00   50
 20  \w     43.00  68.00   0.50    7.00    --  111.50 -61.00-120.00   50
 21  \w     41.00  66.00   0.50    7.00    --  111.50 -61.00 150.00   50
 22  \w     41.00  84.00   0.50    7.00    --  111.50 -77.00-120.00   86
 23  \w     43.00  68.00   0.50    7.00    --  111.50 -61.00  60.00   50
 24  \w     56.00  81.00   0.50    7.00    --  111.50 -77.00 120.00   50
 25  \w     41.00  66.00   0.50    7.00    --  111.50 -61.00   0.00   50
 26  \w     43.00  68.00   0.50    7.00    --  111.50 -61.00 120.00   50
 27  \w     60.00 106.00   0.50    7.00    --  111.50 -91.00 -22.00   92
;
_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      0.1136529000
_diffrn_orient_matrix_UB_12      -0.0217477000
_diffrn_orient_matrix_UB_13      0.0484024000
_diffrn_orient_matrix_UB_21      0.0659236000
_diffrn_orient_matrix_UB_22      0.0368961000
_diffrn_orient_matrix_UB_23      0.0122872000
_diffrn_orient_matrix_UB_31      0.0073764000
_diffrn_orient_matrix_UB_32      0.0055004000
_diffrn_orient_matrix_UB_33      0.1087888000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            37141
_diffrn_reflns_point_group_measured_fraction_full 0.98
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        66.0
_diffrn_reflns_theta_max         80.348
_diffrn_reflns_theta_min         3.652
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.537
_exptl_absorpt_correction_T_max  0.90174
_exptl_absorpt_correction_T_min  0.78805
_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    1.289
_exptl_crystal_description       Needle
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.051
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         12061
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0728P)^2^+5.5020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1294
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10919
_reflns_number_total             12061
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cp05237g2.cif
_cod_data_source_block           pk14try2
_cod_depositor_comments
'Adding full bibliography for 7246057--7246058.cif.'
_cod_database_code               7246058
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C232 H248 Cu8 N16 O16 S16 '
_chemical_oxdiff_usercomment     'from Kaspars'
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.658
_diffrn_oxdiff_digest_frames
;
01fdd69640e246a74b6963b73ddf46cf2e000286d18
;
_diffrn_oxdiff_digest_hkl
;
010df181f85ff925b7c481fd99248321406ede
;
_reflns_odcompleteness_completeness 92.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C53(0.55) H53A(0.55) H53B(0.55) H53C(0.55) C54(0.55) H54A(0.55)
 H54B(0.55) H54C(0.55) C53'(0.45) H53D(0.45) H53E(0.45) H53F(0.45) C54'(0.45)
 H54D(0.45) H54E(0.45) H54F(0.45) C1S(0.5) H1SA(0.5) H1SB(0.5) C2S(0.5)
 H2S(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5) C5S(0.5)
 H5SA(0.5) H5SB(0.5) H5SC(0.5)
3.a Riding coordinates:
 C52(H52)
3.b Ternary CH refined with riding coordinates:
 C22(H22), C25(H25), C55(H55)
3.c Secondary CH2 refined with riding coordinates:
 C3S(H3SA,H3SB), C4S(H4SA,H4SB)
3.d Me refined with riding coordinates:
 C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C53'(H53D,H53E,H53F), C54'(H54D,
 H54E,H54F), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C5S(H5SA,H5SB,H5SC)
3.e Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C18(H18),
 C19(H19), C20(H20), C31(H31), C32(H32), C33(H33), C34(H34), C36(H36), C37(H37),
  C38(H38), C39(H39), C48(H48), C49(H49), C50(H50), C2S(H2S)
3.f X=CH2 refined with riding coordinates:
 C1S(H1SA,H1SB)
3.g Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C58(H58A,H58B,H58C), C59(H59A,
 H59B,H59C)
;
_shelx_res_checksum              39724
_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 1.238
_oxdiff_exptl_absorpt_empirical_full_min 0.734