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_7045597
_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 H32 Ag2 N6 O3, 2(C F3 O3 S), C2 H3 N'
_chemical_formula_sum            'C50 H35 Ag2 F6 N7 O9 S2'
_chemical_formula_weight         1271.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-09-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2017-09-04 deposited with the CCDC.
2018-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.9233(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.72079(13)
_cell_length_b                   30.3305(3)
_cell_length_c                   13.47657(15)
_cell_measurement_reflns_used    24052
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.2380
_cell_measurement_theta_min      2.9070
_cell_volume                     4789.01(10)
_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, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2303
_diffrn_detector_type            AtlasS2
_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   -120.00  -5.00   1.00    1.00    --  -41.77 -19.00 150.00  115
  2  \w    -64.00  31.00   1.00    1.00    --  -41.77  38.00 120.00   95
  3  \w     23.00  97.00   1.00    1.00    --   41.77-125.00-150.00   74
  4  \w    100.00 178.00   1.00    1.40    --  111.00 111.00 -30.00   78
  5  \w     36.00 116.00   1.00    1.40    --  111.00-111.00 -60.00   80
  6  \w     36.00 116.00   1.00    1.40    --  111.00-111.00 120.00   80
  7  \w     80.00 178.00   1.00    1.40    --  111.00  77.00-150.00   98
  8  \w     36.00 116.00   1.00    1.40    --  111.00-111.00  30.00   80
  9  \w     83.00 178.00   1.00    1.40    --  111.00  61.00  30.00   95
 10  \w     30.00 109.00   1.00    1.40    --  111.00 -94.00-180.00   79
 11  \w     83.00 178.00   1.00    1.40    --  111.00  61.00 -30.00   95
 12  \w     30.00 109.00   1.00    1.40    --  111.00 -94.00  30.00   79
 13  \w     36.00 112.00   1.00    1.40    --  111.00-111.00 -90.00   76
 14  \w     77.00 151.00   1.00    1.40    --  111.00 178.00  90.00   74
 15  \w    132.00 176.00   1.00    1.40    --  111.00 111.00-180.00   44
 16  \w    104.00 178.00   1.00    1.40    --  111.00 111.00-120.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0248522000
_diffrn_orient_matrix_UB_12      -0.0474044000
_diffrn_orient_matrix_UB_13      0.0440429000
_diffrn_orient_matrix_UB_21      0.0631173000
_diffrn_orient_matrix_UB_22      0.0182452000
_diffrn_orient_matrix_UB_23      0.1147003000
_diffrn_orient_matrix_UB_31      -0.1127382000
_diffrn_orient_matrix_UB_32      -0.0001906000
_diffrn_orient_matrix_UB_33      0.0173766000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            40177
_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         76.415
_diffrn_reflns_theta_min         2.914
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.168
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.165
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_description       block
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.202
_exptl_crystal_size_min          0.119
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         9982
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+2.8073P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0792
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9595
_reflns_number_total             9982
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04744d2.cif
_cod_data_source_block           mc188
_cod_depositor_comments
'Adding full bibliography for 7045596--7045600.cif.'
_cod_database_code               7045597
_chemical_oxdiff_formula         'C200 H140 Ag8 F24 N28 O36 S8'
_chemical_oxdiff_usercomment     'MC202 CF Symm QPyOHQ + AgOTf ex MeCN/Et2O'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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.a Rotating group:
 O9(H9A)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C11(H11), C13(H13), C16(H16),
 C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27),
  C28(H28), C30(H30), C31(H31), C34(H34), C36(H36), C39(H39), C40(H40),
 C42(H42), C43(H43), C44(H44), C45(H45)
2.c Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C)
2.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2A)
;
_shelx_res_checksum              20176
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2017-07-20
_olex2_exptl_crystal_mounting_method
'mounted on a Mitegen loop using Paratone-N oil'
_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 1.660
_oxdiff_exptl_absorpt_empirical_full_min 0.628