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_4003617
_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         'C28 H41 Ag Cl N'
_chemical_formula_sum            'C28 H41 Ag Cl N'
_chemical_formula_weight         534.94
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.1400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0759(2)
_cell_length_b                   11.7337(2)
_cell_length_c                   21.2836(3)
_cell_measurement_reflns_used    34406
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.1270
_cell_measurement_theta_min      1.9650
_cell_volume                     2516.30(7)
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(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 0.891
_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     19.00  78.00   0.50    0.51    --    4.95  38.00 -39.00  118
  2  \w     38.00  64.00   0.50    0.51    --   -5.49  38.00 -39.00   52
  3  \w    -19.00  16.00   0.50    0.51    --   -5.49  38.00 -39.00   70
  4  \w    -55.00  18.00   0.50    0.51    --    4.95 -34.00  45.38  146
  5  \w    -22.00  28.00   0.50    0.51    --   -5.49 -99.00 120.00  100
  6  \w    -45.00  17.00   0.50    0.51    --    4.95 -38.00 164.00  124
  7  \w    -49.00 -20.00   0.50    0.51    --   -5.49 -38.00 164.00   58
  8  \w    -59.00  18.00   0.50    0.51    --    4.95 -34.00 108.64  154
  9  \w    -65.00  18.00   0.50    0.51    --    4.95 -34.00 -11.35  166
 10  \w    -20.00  28.00   0.50    0.51    --   -5.49 -99.00 -60.00   96
 11  \w    -66.00  18.00   0.50    0.51    --    4.95 -34.00 -76.34  168
 12  \w    -68.00  18.00   0.50    0.51    --    4.95 -33.00-134.75  172
 13  \w    -80.00   1.00   0.50    0.51    --   -5.49 -19.00   0.00  162
;
_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      -0.0588133000
_diffrn_orient_matrix_UB_12      -0.0304292000
_diffrn_orient_matrix_UB_13      0.0072517000
_diffrn_orient_matrix_UB_21      0.0384476000
_diffrn_orient_matrix_UB_22      -0.0435363000
_diffrn_orient_matrix_UB_23      0.0142915000
_diffrn_orient_matrix_UB_31      -0.0040083000
_diffrn_orient_matrix_UB_32      0.0288561000
_diffrn_orient_matrix_UB_33      0.0292298000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            67838
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.914
_diffrn_reflns_theta_min         1.914
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80703
_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    1.412
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.48
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.00070(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         7096
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0269
_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^)+(0.0311P)^2^+2.3525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0694
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6582
_reflns_number_total             7096
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c01769_si_003.cif
_cod_data_source_block           vs_agcl6
_cod_database_code               4003617
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C28H41NClAg
_chemical_oxdiff_usercomment     'DCM/iso-Pentane, light yellow block'
_shelx_estimated_absorpt_t_max   0.666
_shelx_estimated_absorpt_t_min   0.533
_diffrn_oxdiff_digest_frames
;
014e9b3870a121300209b07fa96021684600034cf75
;
_diffrn_oxdiff_digest_hkl
;
016188b952fe92774104b3b406c7cb6b65a710
;
_reflns_odcompleteness_completeness 99.96
_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), C24(H24), C26(H26)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C21(H21A,H21B), C23(H23A,H23B), C25(H25A,H25B),
 C27(H27A,H27B), C28(H28A,H28B)
2.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10)
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), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              31371
_shelx_hkl_checksum              63496
_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 1.188
_oxdiff_exptl_absorpt_empirical_full_min 0.783