Mono- versus Bicyclic Carbene Metal Amide Photoemitters: Which Design Leads to the Best Performance?
Chotard, Florian; Sivchik, Vasily; Linnolahti, Mikko; Bochmann, Manfred; Romanov, Alexander S.; Chemistry of Materials  (2020) –; doi:10.1021/acs.chemmater.0c01769

data_4003622
_publ_section_title
;
 Mono- versus Bicyclic Carbene Metal Amide Photoemitters: Which Design
 Leads to the Best Performance?
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.0c01769
_journal_year                    2020
_chemical_formula_moiety         'C36 H45 Au N2'
_chemical_formula_sum            'C36 H45 Au N2'
_chemical_formula_weight         702.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'intrinsic phasing'
_audit_creation_date             2019-11-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.148(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.0559(6)
_cell_length_b                   13.3859(2)
_cell_length_c                   16.9937(3)
_cell_measurement_reflns_used    25039
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.6610
_cell_measurement_theta_min      2.1380
_cell_volume                     6879.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_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      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.856
_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     -8.00  80.00   0.50   17.27    --    4.95  19.00 150.00  176
  2  \w     -2.00  28.00   0.50   17.27    --   -5.34 -99.00 -30.00   60
  3  \w     -3.00  28.00   0.50   17.27    --    4.95 -77.00 -90.00   62
  4  \w     18.00  77.00   0.50   17.27    --    4.95   0.00-120.00  118
  5  \w    -17.00  10.00   0.50   17.27    --    4.95  77.00 -60.00   54
  6  \w    -18.00  13.00   0.50   17.27    --    4.95  77.00-150.00   62
  7  \w    -37.00  -5.00   0.50   17.27    --    4.95   0.00-120.00   64
  8  \w    -46.00  -1.00   0.50   17.27    --   -5.34 -57.00 -90.00   90
  9  \w    -18.00  28.00   0.50   17.27    --    4.95 -77.00-150.00   92
 10  \w    -20.00  26.00   0.50   17.27    --    4.95 -77.00   0.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  '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      -0.0219008000
_diffrn_orient_matrix_UB_12      -0.0031842000
_diffrn_orient_matrix_UB_13      -0.0238105000
_diffrn_orient_matrix_UB_21      0.0082964000
_diffrn_orient_matrix_UB_22      -0.0148061000
_diffrn_orient_matrix_UB_23      -0.0338251000
_diffrn_orient_matrix_UB_31      -0.0010446000
_diffrn_orient_matrix_UB_32      -0.0507967000
_diffrn_orient_matrix_UB_33      0.0112761000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.856
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            49796
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.856
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.809
_diffrn_reflns_theta_min         1.976
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.301
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53312
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       block
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.244
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.061
_refine_diff_density_max         1.645
_refine_diff_density_min         -1.031
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         9240
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0262
_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^)+(0.0362P)^2^+2.7627P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0644
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7635
_reflns_number_total             9240
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c01769_si_003.cif
_cod_data_source_block           bicaacAucz_1_sq
_cod_database_code               4003622
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C25H30N2Au
_chemical_oxdiff_usercomment     'CD2Cl2/Pet ether, -20d egC; 100K'
_shelx_estimated_absorpt_t_max   0.779
_shelx_estimated_absorpt_t_min   0.420
_diffrn_oxdiff_digest_frames
;
010ca6c28b6e5cfaab8818875b36f1338d00025b7fd
;
_diffrn_oxdiff_digest_hkl
;
0162224ced28a6d9ab8a03f6e32cd60118517c
;
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C20(H20), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C19(H19A,H19B)
2.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C26(H26), C27(H27), C28(H28), C29(H29), C32(H32),
 C33(H33), C34(H34), C35(H35)
2.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C)
;
_shelx_res_checksum              13616
_shelx_hkl_checksum              15953
_shelx_fab_checksum              10341
_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 1.510
_oxdiff_exptl_absorpt_empirical_full_min 0.718