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_8000423
_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_absolute_configuration ad
_chemical_formula_moiety         'C24 H18 Cu3 N9'
_chemical_formula_sum            'C24 H18 Cu3 N9'
_chemical_formula_weight         623.34
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-22
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5484)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   25.6853(11)
_cell_length_b                   10.4956(3)
_cell_length_c                   35.037(2)
_cell_measurement_reflns_used    2040
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      54.0470
_cell_measurement_theta_min      3.6360
_cell_volume                     9445.4(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4098
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details
;
  1 omega  -95.00  -12.60   0.8000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5552  -57.0000  -60.0000 103

  2 omega  -43.00   23.40   0.8000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5552   38.0000  -90.0000 83

  3 omega   35.00   86.20   0.8000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7812  -30.0000   30.0000 64

  4 omega   33.00  114.60   0.8000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7812 -125.0000  150.0000 102

  5 omega   99.00  170.20   0.8000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7812   45.0000 -150.0000 89

  6 omega  109.00  173.00   0.8000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7812  125.0000    0.0000 80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0269918000
_diffrn_orient_matrix_UB_12      0.0020353000
_diffrn_orient_matrix_UB_13      0.0392397000
_diffrn_orient_matrix_UB_21      -0.0534551000
_diffrn_orient_matrix_UB_22      0.0105485000
_diffrn_orient_matrix_UB_23      0.0197048000
_diffrn_orient_matrix_UB_31      -0.0034830000
_diffrn_orient_matrix_UB_32      -0.1464251000
_diffrn_orient_matrix_UB_33      0.0019735000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0700
_diffrn_reflns_av_unetI/netI     0.1032
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            22363
_diffrn_reflns_point_group_measured_fraction_full 0.744
_diffrn_reflns_point_group_measured_fraction_max 0.712
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.188
_diffrn_reflns_theta_min         3.441
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.411
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_description       column
_exptl_crystal_F_000             4996
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.31(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1298
_refine_ls_number_reflns         13689
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.1347
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.1196
_reflns_Friedel_coverage         0.452
_reflns_Friedel_fraction_full    0.488
_reflns_Friedel_fraction_max     0.451
_reflns_number_gt                6414
_reflns_number_total             13689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jz9b03382_si_002.cif
_cod_data_source_block           Cu-2-293K
_cod_depositor_comments
;

2025-04-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C96 H73 Cu12 N36'
_cod_original_formula_weight         2493.38
_cod_original_formula_moiety         'C48 H37 Cu6 N18, C48 H36 Cu6 N18'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        9445.3(8)
_cod_database_code               8000423
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C N H Cu'
_reflns_odcompleteness_completeness 98.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.29
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.69(6)
 0.31(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
3. Rigid bond restraints
 N10, C29
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C37, C38
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C57, C58
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C69, C70
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Aromatic/amide H refined with riding coordinates:
 C92(H92), C32(H32), C80(H80), C88(H88), C89(H89), C74(H74), C96(H96),
 C31(H31), C84(H84), C75(H75), C73(H73), C81(H81), C17(H17), C79(H79), C16(H16),
  C82(H82), C44(H44), C51(H51), C90(H90), C48(H48), C63(H63), C20(H20),
 C76(H76), C83(H83), C9(H9), C87(H87), C18(H18), C15(H15), C7(H7), C8(H8),
 C23(H23), C95(H95), C52(H52), C47(H47), C24(H24), C11(H11), C56(H56), C64(H64),
  C19(H19), C4(H4), C41(H41), C50(H50), C49(H49), C28(H28), C57(H57), C1(H1),
 C71(H71), C10(H10), C91(H91), C12(H12), C67(H67), C39(H39), C40(H40), C68(H68),
  C59(H59), C58(H58), C33(H33), C3(H3), C72(H72), N10(H10A), C35(H35), C60(H60),
  C42(H42), C43(H43), C2(H2), C36(H36), C34(H34), C55(H55), C65(H65), C66(H66),
 C26(H26), C25(H25), C27(H27)
;
_shelx_res_checksum              80224
_shelx_hkl_checksum              34575
_olex2_submission_special_instructions 'No special instructions were received'