Revealing High-Lying Inter-System Crossing in Brightly Luminescent Cyclic Trinuclear Cu<sup>I</sup>/Ag<sup>I</sup> Complexes.
Xing, Li-Rui; Lu, Zhou; Li, Mian; Zheng, Ji; Li, Dan; The journal of physical chemistry letters  (2020) 2067–; doi:10.1021/acs.jpclett.9b03382

data_8000427
_publ_section_title
;
 Revealing High-Lying Inter-System Crossing in Brightly Luminescent Cyclic
 Trinuclear Cu<sup>I</sup>/Ag<sup>I</sup> Complexes.
;
_journal_name_full               'The journal of physical chemistry letters'
_journal_page_first              2067
_journal_paper_doi               10.1021/acs.jpclett.9b03382
_journal_year                    2020
_chemical_formula_moiety         '2(C12 H9 Cu1.5 N4.5)'
_chemical_formula_sum            'C24 H18 Cu3 N9'
_chemical_formula_weight         623.09
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-23
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_cell_angle_alpha                89.557(2)
_cell_angle_beta                 80.608(4)
_cell_angle_gamma                89.749(4)
_cell_formula_units_Z            4
_cell_length_a                   7.2140(4)
_cell_length_b                   18.8723(5)
_cell_length_c                   19.0253(5)
_cell_measurement_reflns_used    9686
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.3490
_cell_measurement_theta_min      4.7240
_cell_volume                     2555.38(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2013/2 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.964
_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     48.00  81.00   0.50    0.50    --    0.00  57.00  30.00   66
  2  \w     18.00  49.00   0.50    0.50    --    0.00  57.00-180.00   62
  3  \w      9.00  43.00   0.50    0.50    --    0.00  57.00  30.00   68
  4  \w    -29.00  84.00   0.50    0.50    --    0.00  57.00 -60.00  226
  5  \w     61.00  96.00   0.50    3.00    --   94.60  30.00 120.00   70
  6  \w    104.00 130.00   0.50    3.00    --   94.60  30.00 120.00   52
  7  \w     67.00 183.00   0.50    3.00    --   94.60  45.00 150.00  232
  8  \w    155.00 181.00   0.50    3.00    --   94.60  61.00-120.00   52
  9  \w    102.00 128.00   0.50    3.00    --   94.60 -30.00-150.00   52
 10  \w     94.00 121.00   0.50    3.00    --   94.60 -82.00   0.00   54
 11  \w     69.00 101.00   0.50    3.00    --   94.60 -82.00 -90.00   64
 12  \w     73.00  99.00   0.50    3.00    --   94.60 -82.00-150.00   52
 13  \w     73.00 101.00   0.50    3.00    --   94.60 -77.00-150.00   56
 14  \w     44.00  70.00   0.50    3.00    --   94.60 -82.00-180.00   52
 15  \w     39.00 130.00   0.50    3.00    --   94.60 -82.00 -60.00  182
 16  \w     73.00 131.00   0.50    3.00    --   94.60 -82.00 120.00  116
 17  \w     75.00 175.00   0.50    3.00    --   94.60  45.00-180.00  200
 18  \w     65.00  96.00   0.50    3.00    --   94.60  61.00-120.00   62
 19  \w     11.00  85.00   0.50    3.00    --   94.60 -30.00-150.00  148
 20  \w     12.00 123.00   0.50    3.00    --   94.60 -61.00  30.00  222
 21  \w     12.00 119.00   0.50    3.00    --   94.60 -82.00  90.00  214
 22  \w      5.00 103.00   0.50    3.00    --   94.60 -61.00 -60.00  196
 23  \w     11.00  86.00   0.50    3.00    --   94.60 -45.00-150.00  150
 24  \w    -88.00  19.00   0.50    0.50    --    0.00 -38.00 -60.00  214
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0176729000
_diffrn_orient_matrix_UB_12      0.0287830000
_diffrn_orient_matrix_UB_13      0.0763657000
_diffrn_orient_matrix_UB_21      -0.0494023000
_diffrn_orient_matrix_UB_22      -0.0748134000
_diffrn_orient_matrix_UB_23      0.0300789000
_diffrn_orient_matrix_UB_31      0.2099991000
_diffrn_orient_matrix_UB_32      -0.0154443000
_diffrn_orient_matrix_UB_33      -0.0003001000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27125
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.200
_diffrn_reflns_theta_min         3.309
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.152
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_meas      1.620
_exptl_crystal_description       needle
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         9993
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0808P)^2^+0.0931P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1410
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7580
_reflns_number_total             9993
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jz9b03382_si_002.cif
_cod_data_source_block           Cu-4-293K
_cod_database_code               8000427
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid body (RIGU) restrains
 N20, C52, C47, C53, C41, C43
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C49, N19, C33, C14, C37, C50
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C37, C44, C45, N17, C33, C14
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N18, C51, C46, C48, C41, C43
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Fixed Sof: H33A(0.75) H33(0.25) H41A(0.75) H41(0.25) N17(0.75) H43A(0.75)
 H43(0.25) C44(0.75) H44(0.75) N18(0.75) C45(0.75) H45(0.75) C46(0.75)
 H46(0.75) C47(0.25) H47(0.25) C48(0.75) C49(0.25) H49(0.25) C50(0.25)
 H50(0.25) N19(0.25) C51(0.75) H51(0.75) N20(0.25) C52(0.25) H52(0.25) C53(0.25)
4.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16),
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33A),
 C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40),
 C41(H41A), C41(H41), C42(H42), C43(H43A), C43(H43), C44(H44), C45(H45),
 C46(H46), C47(H47), C49(H49), C50(H50), C51(H51), C52(H52)
;
_smtbx_masks_void_probe_radius   0.5
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              57327
_shelx_hkl_checksum              27389
_shelx_fab_checksum              22687
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.675
_oxdiff_exptl_absorpt_empirical_full_min 0.607