Self-assembly of singlet-emitting double-helical silver dimers: the curious coordination chemistry and fluorescence of bisquinolylpyridone.
Farrow, Charlotte M. A.; Akien, Geoffrey R.; Halcovitch, Nathan R.; Platts, James A.; Coogan, M. P.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 3906–3912; doi:10.1039/c7dt04744d

data_7045599
_publ_section_title
;
 Self-assembly of singlet-emitting double-helical silver dimers: the
 curious coordination chemistry and fluorescence of bisquinolylpyridone.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3906
_journal_page_last               3912
_journal_paper_doi               10.1039/c7dt04744d
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '4(C23 H15 N3 O)'
_chemical_formula_sum            'C92 H60 N12 O4'
_chemical_formula_weight         1397.52
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-01-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-01-17 deposited with the CCDC.
2018-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                104.8568(17)
_cell_angle_beta                 105.8861(17)
_cell_angle_gamma                105.3698(17)
_cell_formula_units_Z            2
_cell_length_a                   11.5071(2)
_cell_length_b                   17.7155(4)
_cell_length_c                   19.7489(4)
_cell_measurement_reflns_used    25527
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.4380
_cell_measurement_theta_min      2.9450
_cell_volume                     3490.88(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.44a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.44a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.44a (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_temperature      100(2)
_diffrn_detector_area_resol_mean 5.2303
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_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   -112.00 -15.00   1.00    2.00    --  -41.77 -57.00  60.00   97
  2  \w    -64.00  31.00   1.00    2.00    --  -41.77  38.00   0.00   95
  3  \w    -68.00  28.00   1.00    2.00    --  -41.77  57.00-150.00   96
  4  \w      1.00  82.00   1.00    2.00    --   41.77 -99.00 -90.00   81
  5  \w      1.00  82.00   1.00    2.00    --   41.77 -99.00   0.00   81
  6  \w     36.00 116.00   1.00    8.00    --  111.00-111.00-180.00   80
  7  \w     83.00 178.00   1.00    8.00    --  111.00  61.00  30.00   95
  8  \w     37.00 142.00   1.00    8.00    --  111.00 -77.00-180.00  105
  9  \w     57.00 151.00   1.00    8.00    --  111.00 178.00 -60.00   94
 10  \w     36.00 116.00   1.00    8.00    --  111.00-111.00   0.00   80
 11  \w     37.00 142.00   1.00    8.00    --  111.00 -77.00   0.00  105
 12  \w     80.00 178.00   1.00    8.00    --  111.00  77.00-150.00   98
 13  \w     36.00 116.00   1.00    8.00    --  111.00-111.00  60.00   80
 14  \w     87.00 178.00   1.00    8.00    --  111.00  45.00 -30.00   91
 15  \w     57.00 151.00   1.00    8.00    --  111.00 178.00-180.00   94
 16  \w     36.00 116.00   1.00    8.00    --  111.00-111.00 150.00   80
 17  \w     36.00 116.00   1.00    8.00    --  111.00-111.00 -90.00   80
 18  \w     83.00 178.00   1.00    8.00    --  111.00  61.00-180.00   95
 19  \w     30.00 109.00   1.00    8.00    --  111.00 -94.00 -90.00   79
 20  \w     30.00 109.00   1.00    8.00    --  111.00 -94.00-180.00   79
 21  \w     83.00 178.00   1.00    8.00    --  111.00  61.00  60.00   95
 22  \w    100.00 178.00   1.00    8.00    --  111.00 111.00-120.00   78
 23  \w     80.00 178.00   1.00    8.00    --  111.00  77.00 -90.00   98
 24  \w     30.00 109.00   1.00    8.00    --  111.00 -94.00 -30.00   79
 25  \w     87.00 178.00   1.00    8.00    --  111.00  45.00 150.00   91
 26  \w     36.00 116.00   1.00    8.00    --  111.00-111.00 120.00   80
 27  \w     83.00 178.00   1.00    8.00    --  111.00  61.00-120.00   95
 28  \w    100.00 178.00   1.00    8.00    --  111.00 111.00 120.00   78
 29  \w   -112.00 -19.00   1.00    2.00    --  -41.77 -57.00-120.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            58230
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.786
_diffrn_reflns_theta_min         2.488
_exptl_absorpt_coefficient_mu    0.665
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.44a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       plate
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.349
_exptl_crystal_size_mid          0.219
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1054
_refine_ls_number_reflns         14565
_refine_ls_number_restraints     197
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0665P)^2^+1.1202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1294
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12534
_reflns_number_total             14565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04744d2.cif
_cod_data_source_block           mc186
_cod_depositor_comments
'Adding full bibliography for 7045596--7045600.cif.'
_cod_original_cell_volume        3490.89(13)
_cod_database_code               7045599
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 N3D-C15D \\sim N3E-C15E
 with sigma of 0.02
 N3D-C23D \\sim N3E-C23E
 with sigma of 0.02
 C14D-C15D \\sim C14D-C15E
 with sigma of 0.02
 C15D-C16D \\sim C15E-C16E
 with sigma of 0.02
 C23D-C18D \\sim C23E-C18E
 with sigma of 0.02
 C23D-C22D \\sim C23E-C22E
 with sigma of 0.02
 C18D-C19D \\sim C18E-C19E
 with sigma of 0.02
 C18D-C17D \\sim C18E-C17E
 with sigma of 0.02
 C19D-C20D \\sim C19E-C20E
 with sigma of 0.02
 C20D-C21D \\sim C20E-C21E
 with sigma of 0.02
 C21D-C22D \\sim C21E-C22E
 with sigma of 0.02
 C16D-C17D \\sim C16E-C17E
 with sigma of 0.02
 N3D-C14D \\sim N3E-C14D
 with sigma of 0.04
 N3D-C18D \\sim N3E-C18E
 with sigma of 0.04
 N3D-C22D \\sim N3E-C22E
 with sigma of 0.04
 N3D-C16D \\sim N3E-C16E
 with sigma of 0.04
 C14D-C16D \\sim C14D-C16E
 with sigma of 0.04
 C15D-C23D \\sim C15E-C23E
 with sigma of 0.04
 C15D-C17D \\sim C15E-C17E
 with sigma of 0.04
 C23D-C19D \\sim C23E-C19E
 with sigma of 0.04
 C23D-C21D \\sim C23E-C21E
 with sigma of 0.04
 C23D-C17D \\sim C23E-C17E
 with sigma of 0.04
 C18D-C20D \\sim C18E-C20E
 with sigma of 0.04
 C18D-C22D \\sim C18E-C22E
 with sigma of 0.04
 C18D-C16D \\sim C18E-C16E
 with sigma of 0.04
 C19D-C21D \\sim C19E-C21E
 with sigma of 0.04
 C19D-C17D \\sim C19E-C17E
 with sigma of 0.04
 C20D-C22D \\sim C20E-C22E
 with sigma of 0.04
3. Restrained planarity
 N3E, C15E, C23E, C18E, C20E, C21E, C22E, C16E, C17E, C19E
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
N3D \\sim N3E: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C22D \\sim C22E: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
5. Rigid body (RIGU) restrains
 N3D, C15D, C23D, C18D, C19D, C20D, C21D, C22D, C16D, C17D
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N3E, C15E, C23E, C18E, C19E, C20E, C21E, C22E, C16E, C17E
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(N3E)=Sof(C15E)=Sof(C23E)=Sof(C18E)=Sof(C19E)=Sof(H19E)=Sof(C20E)=
 Sof(H20E)=Sof(C21E)=Sof(H21E)=Sof(C22E)=Sof(H22E)=Sof(C16E)=Sof(H16E)=
 Sof(C17E)=Sof(H17E)=1-FVAR(1)
 Sof(N3D)=Sof(C15D)=Sof(C23D)=Sof(C18D)=Sof(C19D)=Sof(H19D)=Sof(C20D)=
 Sof(H20D)=Sof(C21D)=Sof(H21D)=Sof(C22D)=Sof(H22D)=Sof(C16D)=Sof(H16D)=
 Sof(C17D)=Sof(H17D)=FVAR(1)
7.a Aromatic/amide H refined with riding coordinates:
 N2B(H2B), N2C(H2C), C11B(H11B), C13(H13), C13B(H13B), C8B(H8B), C11(H11),
 C16B(H16B), C2B(H2BA), C7B(H7B), C16(H16), C2C(H2CA), C8(H8), C13C(H13C),
 C17B(H17B), C16C(H16C), C22B(H22B), C8C(H8C), C11D(H11D), C11C(H11C), C3B(H3B),
  C4B(H4B), C19C(H19C), C19(H19), C22C(H22C), C13D(H13D), C7(H7), C7C(H7C),
 C21C(H21C), C5B(H5B), C17C(H17C), C3C(H3C), C20C(H20C), C19B(H19B), C17(H17),
 C22(H22), C21B(H21B), C2(H2), C4C(H4C), C5(H5), C3(H3), C5C(H5C), C20(H20),
 C2D(H2D), C20B(H20B), C21(H21), C19D(H19D), C20D(H20D), C21D(H21D), C22D(H22D),
  C8D(H8D), C4(H4), C7D(H7D), C3D(H3D), C4D(H4D), C5D(H5D), C16D(H16D),
 C17D(H17D), C19E(H19E), C20E(H20E), C21E(H21E), C22E(H22E), C16E(H16E),
 C17E(H17E)
7.b Fitted hexagon refined as free rotating group:
 C23D(C18D,C19D,C20D,C21D,C22D)
7.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O1D(H1D)
;
_shelx_res_checksum              47323
_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
;