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_7045600
_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
'C46 H30 Ag2 N6 O2, 2(B F4), 0.5(C2 H3 N), 0.5(O)'
_chemical_formula_sum            'C47 H31.5 Ag2 B2 F8 N6.5 O2.5'
_chemical_formula_weight         1116.65
_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                87.526(3)
_cell_angle_beta                 80.106(3)
_cell_angle_gamma                85.894(3)
_cell_formula_units_Z            4
_cell_length_a                   13.5216(5)
_cell_length_b                   14.9223(6)
_cell_length_c                   21.6131(8)
_cell_measurement_reflns_used    15538
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.0540
_cell_measurement_theta_min      3.5770
_cell_volume                     4282.9(3)
_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 0.995
_diffrn_measured_fraction_theta_max 0.971
_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   -114.00 -19.00   1.00    7.50    --  -41.77 -38.00  30.00   95
  2  \w   -120.00  -5.00   1.00    7.50    --  -41.77 -19.00 120.00  115
  3  \w    -64.00  31.00   1.00    7.50    --  -41.77  38.00  30.00   95
  4  \w      1.00  82.00   1.00    7.50    --   41.77 -99.00 120.00   81
  5  \w     23.00  97.00   1.00    7.50    --   41.77-125.00  30.00   74
  6  \w     10.00 116.00   1.00    7.50    --   41.77  77.00-120.00  106
  7  \w     87.00 178.00   1.00   30.00    --  111.00  30.00 -30.00   91
  8  \w     36.00 116.00   1.00   30.00    --  111.00-111.00 150.00   80
  9  \w     37.00 142.00   1.00   30.00    --  111.00 -77.00-180.00  105
 10  \w     87.00 178.00   1.00   30.00    --  111.00  45.00 -90.00   91
 11  \w     83.00 178.00   1.00   30.00    --  111.00  61.00-180.00   95
 12  \w     40.00 135.00   1.00   30.00    --  111.00 -45.00-180.00   95
 13  \w     40.00 135.00   1.00   30.00    --  111.00 -45.00 -60.00   95
 14  \w     36.00 116.00   1.00   30.00    --  111.00-111.00 -60.00   80
 15  \w     66.00 178.00   1.00   30.00    --  111.00  15.00 -90.00  112
 16  \w     36.00 116.00   1.00   30.00    --  111.00-111.00-150.00   80
 17  \w     36.00 116.00   1.00   30.00    --  111.00-111.00  90.00   80
 18  \w     36.00 116.00   1.00   30.00    --  111.00-111.00 -30.00   80
 19  \w     41.00 139.00   1.00   30.00    --  111.00 -61.00  90.00   98
 20  \w     30.00 109.00   1.00   30.00    --  111.00 -94.00   0.00   79
 21  \w     87.00 166.00   1.00   30.00    --  111.00  45.00-150.00   79
;
_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  0.0348
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            49184
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.680
_diffrn_reflns_theta_min         2.970
_exptl_absorpt_coefficient_mu    8.088
_exptl_absorpt_correction_T_max  0.798
_exptl_absorpt_correction_T_min  0.487
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.44a (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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_description       block
_exptl_crystal_F_000             2220
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.059
_refine_diff_density_max         3.249
_refine_diff_density_min         -1.964
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1240
_refine_ls_number_reflns         17514
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+19.3392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1615
_refine_ls_wR_factor_ref         0.1768
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12967
_reflns_number_total             17514
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04744d2.cif
_cod_data_source_block           mc176
_cod_depositor_comments
'Adding full bibliography for 7045596--7045600.cif.'
_cod_original_cell_volume        4283.0(3)
_cod_original_formula_sum        'C47 H31.50 Ag2 B2 F8 N6.50 O2.50'
_cod_database_code               7045600
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 F3-B1 \\sim F4-B1 \\sim F2-B1 \\sim F1-B1
 with sigma of 0.02
3. Others
 Sof(O5A)=1-FVAR(1)
 Sof(O5)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C45(H45), C44(H44), C17(H17), C25(H25), C22(H22), C21(H21), C16(H16),
 C19(H19), C40(H40), C42(H42), C31(H31), C13(H13), C43(H43), C39(H39), C7B(H7B),
  C25B(H25B), C30B(H30B), C36(H36), C31B(H31B), C34(H34), C30(H30), C8(H8),
 C13B(H13B), C2B(H2BA), C20(H20), C36B(H36B), C8B(H8B), C16B(H16B), C3B(H3B),
 C27B(H27B), C26(H26), C26B(H26B), C11(H11), C28B(H28B), C4B(H4B), C11B(H11B),
 C7(H7), C28(H28), C22B(H22B), C2(H2A), C34B(H34B), C17B(H17B), C19B(H19B),
 C27(H27), C40B(H40B), C39B(H39B), C42B(H42B), C5B(H5B), C45B(H45B), C21B(H21B),
  C3(H3), C20B(H20B), C5(H5), C44B(H44B), C4(H4), C43B(H43B)
4.b Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C)
4.c Idealised tetrahedral OH refined as rotating group:
 O2(H2), O1(H1), O1B(H1B), O2B(H2B)
;
_shelx_res_checksum              69312
_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
;