Dinuclear Ag(I) Complex Designed for Highly Efficient Thermally Activated Delayed Fluorescence.
Shafikov, Marsel Z.; Suleymanova, Alfiya F.; Schinabeck, Alexander; Yersin, Hartmut; The journal of physical chemistry letters  (2018) 702–709; doi:10.1021/acs.jpclett.7b03160

data_8000266
_publ_section_title
;
 Dinuclear Ag(I) Complex Designed for Highly Efficient Thermally Activated
 Delayed Fluorescence.
;
_journal_name_full               'The journal of physical chemistry letters'
_journal_page_first              702
_journal_page_last               709
_journal_paper_doi               10.1021/acs.jpclett.7b03160
_journal_year                    2018
_chemical_formula_moiety         'C106 H102 Ag2 B18 P8'
_chemical_formula_sum            'C106 H102 Ag2 B18 P8'
_chemical_formula_weight         2033.95
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2016-11-22
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.0660(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.33900(10)
_cell_length_b                   26.3269(2)
_cell_length_c                   15.16330(10)
_cell_measurement_reflns_used    51060
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      73.4390
_cell_measurement_theta_min      4.2320
_cell_volume                     5311.56(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_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      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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   -117.00 -15.00   1.00    3.50    --  -41.08 -37.00  60.00  102
  2  \w   -115.00 -11.00   1.00    3.50    --  -41.08 -57.00-180.00  104
  3  \w      2.00  98.00   1.00    3.50    --   41.08-125.00  60.00   96
  4  \w     11.00 115.00   1.00    3.50    --   41.08  57.00 -90.00  104
  5  \w    -33.00  71.00   1.00    3.50    --   41.08 -57.00 150.00  104
  6  \w      5.00  33.00   1.00    3.50    --   42.00  88.00 -74.03   28
  7  \w      3.00  29.00   1.00    3.50    --   42.00  91.00  21.63   26
  8  \w     11.00  45.00   1.00    3.50    --   46.00  82.00-176.28   34
  9  \w     19.00  45.00   1.00    3.50    --   54.00  82.00 -15.68   26
 10  \w     19.00  46.00   1.00    3.50    --   54.00  81.00  39.93   27
 11  \w     20.00  47.00   1.00    3.50    --   54.00  79.00 101.58   27
 12  \w     19.00  46.00   1.00    3.50    --   54.00  81.00 -60.14   27
 13  \w     19.00  45.00   1.00    3.50    --   54.00  82.00-123.93   26
 14  \w     33.00 144.00   1.00    3.50    --   66.00  75.00 -77.01  111
 15  \w     32.00 145.00   1.00    3.50    --   66.00  77.00 -14.49  113
 16  \w     33.00 144.00   1.00    3.50    --   66.00  75.00 -77.01  111
 17  \w     36.00 149.00   1.00    3.50    --   70.00  77.00  67.17  113
 18  \w     36.00 149.00   1.00    3.50    --   70.00  77.00-135.01  113
 19  \w     37.00 148.00   1.00    3.50    --   70.00  76.00 108.31  111
 20  \w     37.00 148.00   1.00    3.50    --   70.00  76.00 141.11  111
 21  \w     37.00 148.00   1.00    3.50    --   70.00  76.00  15.79  111
 22  \w     40.00 153.00   1.00    3.50    --   74.00  77.00  38.34  113
 23  \w     49.00 158.00   1.00   12.50    --   82.00  73.00 -69.93  109
 24  \w     55.00 130.00   1.00   12.50    --   86.00  63.00  -7.07   75
 25  \w     45.00  71.00   1.00   12.50    --  106.98 -45.00 -60.00   26
 26  \w     73.00 154.00   1.00   12.50    --  106.98  77.00-150.00   81
 27  \w     78.00 103.00   1.00   12.50    --  106.98  61.00-120.00   25
 28  \w     78.00 136.00   1.00   12.50    --  106.98  61.00-180.00   58
 29  \w     73.00 153.00   1.00   12.50    --  106.98  77.00 -60.00   80
 30  \w    104.00 138.00   1.00   12.50    --  106.98  77.00 150.00   34
 31  \w     32.00 118.00   1.00   12.50    --  106.98-125.00  60.00   86
 32  \w     73.00  98.00   1.00   12.50    --  106.98  77.00 150.00   25
 33  \w     73.00 155.00   1.00   12.50    --  106.98  77.00   0.00   82
 34  \w     23.00  82.00   1.00   12.50    --  106.98 -94.00  60.00   59
 35  \w     42.00  68.00   1.00   12.50    --  106.98 -45.00 120.00   26
 36  \w     73.00 157.00   1.00   12.50    --  106.98  77.00-120.00   84
 37  \w     73.00 143.00   1.00   12.50    --  106.98  77.00-180.00   70
 38  \w     35.00  80.00   1.00   12.50    --  106.98 -94.00-120.00   45
 39  \w     40.00  76.00   1.00   12.50    --  106.98 -45.00-120.00   36
 40  \w     35.00  91.00   1.00   12.50    --  106.98 -94.00 -30.00   56
 41  \w     73.00 152.00   1.00   12.50    --  106.98  77.00  60.00   79
 42  \w     38.00  89.00   1.00   12.50    --  106.98 -94.00 150.00   51
 43  \w     73.00 158.00   1.00   12.50    --  106.98  77.00  30.00   85
 44  \w     73.00 158.00   1.00   12.50    --  106.98  77.00 -90.00   85
 45  \w    103.00 157.00   1.00   12.50    --  106.98  77.00 120.00   54
 46  \w     77.00 102.00   1.00   12.50    --  106.98  61.00 150.00   25
 47  \w     34.00 102.00   1.00   12.50    --  106.98 -94.00  90.00   68
 48  \w     73.00  98.00   1.00   12.50    --  106.98  77.00 120.00   25
 49  \w     73.00 157.00   1.00   12.50    --  106.98  77.00 -30.00   84
 50  \w     39.00  98.00   1.00   12.50    --  106.98 -94.00 -90.00   59
 51  \w     46.00  72.00   1.00   12.50    --  106.98 -45.00  60.00   26
 52  \w     46.00 120.00   1.00   12.50    --  106.98-125.00-120.00   74
 53  \w     73.00 152.00   1.00   12.50    --  106.98  77.00  90.00   79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0082744000
_diffrn_orient_matrix_UB_12      0.0143848000
_diffrn_orient_matrix_UB_13      0.0987259000
_diffrn_orient_matrix_UB_21      0.0248977000
_diffrn_orient_matrix_UB_22      0.0551475000
_diffrn_orient_matrix_UB_23      -0.0244321000
_diffrn_orient_matrix_UB_31      -0.1127854000
_diffrn_orient_matrix_UB_32      0.0132365000
_diffrn_orient_matrix_UB_33      -0.0055838000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            117518
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.540
_diffrn_reflns_theta_min         3.370
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.435
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.809
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       prism
_exptl_crystal_F_000             2084
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         10650
_refine_ls_number_restraints     342
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+3.6519P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0714
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9671
_reflns_number_total             10650
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jz7b03160_si_002.cif
_cod_data_source_block           p184
_cod_database_code               8000266
_chemical_oxdiff_formula         'C106 H102 B18 P8 Ag2'
_chemical_oxdiff_usercomment     Suleymanova_Yersin_AS-132
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
2. Uiso/Uaniso restraints and constraints
C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C45 \\sim C15 \\sim C16 \\sim
C17 \\sim C20 \\sim C18 \\sim C19 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim
C43 \\sim C44 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C9:
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01
3. Others
 Sof(C39)=Sof(C40)=Sof(H40)=Sof(C41)=Sof(H41)=Sof(C42)=Sof(H42)=Sof(C43)=
 Sof(H43)=Sof(C44)=Sof(H44)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=Sof(C12)=
 Sof(H12)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14)=Sof(C9)=1-FVAR(1)
 Sof(C46)=Sof(H46)=Sof(C47)=Sof(H47)=Sof(C48)=Sof(H48)=Sof(C49)=Sof(H49)=
 Sof(C50)=Sof(H50)=Sof(C45)=Sof(C15)=Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17)=
 Sof(C20)=Sof(H20)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C52(H52), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C55(H55),
 C61(H61), C59(H59), C22(H22), C34(H34), C5(H5), C64(H64), C56(H56), C38(H38),
 C28(H28), C62(H62), C26(H26), C37(H37), C4(H4), C16(H16), C35(H35), C6(H6),
 C17(H17), C65(H65), C63(H63), C8(H8), C36(H36), C29(H29), C58(H58), C25(H25),
 C32(H32), C23(H23), C31(H31), C57(H57), C7(H7), C30(H30), C24(H24), C20(H20),
 C18(H18), C19(H19), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C10(H10),
  C11(H11), C12(H12), C13(H13), C14(H14)
4.b Fitted hexagon refined as free rotating group:
 C46(C47,C48,C49,C50,C45), C39(C40,C41,C42,C43,C44), C10(C11,C12,C13,C14,C9)
4.c Boron cage BH refined with riding coordinates:
 B5(H5A), B4(H4A), B6(H6A), B3(H3), B7(H7A), B9(H9)
;
_shelx_fab_checksum              29680
_shelx_shelxl_version_number     2016/6
_olex2_date_sample_data_collection 2016-11-21
_olex2_date_sample_submission    2016-11-15
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems CryoStream 700'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder with inert oil'
_olex2_submission_original_sample_id 'AS-132 '
_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 1.278
_oxdiff_exptl_absorpt_empirical_full_min 0.798