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_4003615
_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 Cl Cu N'
_chemical_formula_sum            'C28 H41 Cl Cu N'
_chemical_formula_weight         490.61
_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
_atom_sites_solution_primary     'intrinsic phasing'
_audit_creation_date             2019-11-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.626(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6940(2)
_cell_length_b                   10.3459(2)
_cell_length_c                   20.8452(4)
_cell_measurement_reflns_used    13641
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.8400
_cell_measurement_theta_min      2.1800
_cell_volume                     2521.81(8)
_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      100.01(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 0.857
_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    -68.00   5.00   0.50   23.54    --    5.10 -19.00 -30.00  146
  2  \w     -7.00  19.00   0.50   23.54    --   -5.49 -99.00 -30.00   52
  3  \w    -23.00  28.00   0.50   23.54    --   -5.49 -99.00   0.00  102
  4  \w    -23.00  11.00   0.50   23.54    --   -5.49 -99.00-120.00   68
  5  \w    -69.00   2.00   0.50   23.54    --    5.10 -19.00-150.00  142
  6  \w    -65.00  23.00   0.50   23.54    --    5.10 -77.00 -60.00  176
  7  \w     -6.00  67.00   0.50   23.54    --    5.10  37.00 150.00  146
;
_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      -0.0359702000
_diffrn_orient_matrix_UB_12      -0.0415073000
_diffrn_orient_matrix_UB_13      0.0178814000
_diffrn_orient_matrix_UB_21      -0.0462385000
_diffrn_orient_matrix_UB_22      0.0434910000
_diffrn_orient_matrix_UB_23      -0.0046219000
_diffrn_orient_matrix_UB_31      -0.0157492000
_diffrn_orient_matrix_UB_32      -0.0329264000
_diffrn_orient_matrix_UB_33      -0.0285859000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.857
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            35669
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.857
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.948
_diffrn_reflns_theta_min         1.954
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52018
_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            'light yellow'
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.403
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.036
_refine_diff_density_max         1.241
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         6853
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0748P)^2^+0.3062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1191
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5463
_reflns_number_total             6853
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c01769_si_003.cif
_cod_data_source_block           vs_6caacCucl
_cod_database_code               4003615
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C32H34NCuCl
_chemical_oxdiff_usercomment     'DCM/hexanes, light yellow block'
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.692
_diffrn_oxdiff_digest_frames
;
01ff564e4d9a0a4f9a252d44756ec3b2fe00025b470
;
_diffrn_oxdiff_digest_hkl
;
01d8801be3e9eba1dcd0d038c5b571b5cd4c1f
;
_reflns_odcompleteness_completeness 99.91
_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:
 C14(H14), C17(H17), C20(H20), C22(H22), C24(H24), C27(H27)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C21(H21A,H21B), C23(H23A,H23B), C25(H25A,H25B),
 C26(H26A,H26B), C28(H28A,H28B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12)
2.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              69454
_shelx_hkl_checksum              70660
_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 1.547
_oxdiff_exptl_absorpt_empirical_full_min 0.481