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_7045598
_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         '2(C23 H15 N3 O)'
_chemical_formula_sum            'C46 H30 N6 O2'
_chemical_formula_weight         698.76
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-08-29
_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                 97.629(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2068(4)
_cell_length_b                   6.07880(19)
_cell_length_c                   30.4579(10)
_cell_measurement_reflns_used    8294
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.1020
_cell_measurement_theta_min      2.6480
_cell_volume                     3341.11(17)
_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      100.00(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 0.985
_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    -67.00  28.00   1.00   15.00    --  -41.77  57.00  90.00   95
  2  \w   -112.00 -16.00   1.00   15.00    --  -41.77 -57.00 -60.00   96
  3  \w     25.00  73.00   1.00   15.00    --   41.77 -77.00 -60.00   48
  4  \w     69.00  96.00   1.00   15.00    --   41.77-125.00  90.00   27
  5  \w     32.00  68.00   1.00   60.00    --  111.00 -94.00-150.00   36
  6  \w     87.00 178.00   1.00   60.00    --  111.00  30.00  60.00   91
  7  \w     78.00 135.00   1.00   60.00    --  111.00 -45.00-120.00   57
  8  \w     54.00  91.00   1.00   60.00    --  111.00 -94.00 -90.00   37
  9  \w     82.00 115.00   1.00   60.00    --  111.00-111.00 120.00   33
 10  \w    101.00 175.00   1.00   60.00    --  111.00 111.00-120.00   74
 11  \w     56.00 116.00   1.00   60.00    --  111.00-111.00-120.00   60
 12  \w     70.00  95.00   1.00   60.00    --  111.00 178.00  90.00   25
 13  \w    112.00 145.00   1.00   60.00    --  111.00 178.00  90.00   33
 14  \w     78.00 142.00   1.00   60.00    --  111.00 178.00-180.00   64
 15  \w     40.00  73.00   1.00   60.00    --  111.00 -45.00-120.00   33
 16  \w    102.00 149.00   1.00   60.00    --  111.00 111.00  30.00   47
 17  \w     59.00 146.00   1.00   60.00    --  111.00 178.00 150.00   87
 18  \w    -31.00  60.00   1.00   15.00    --   41.77 -38.00 150.00   91
 19  \w     10.00 116.00   1.00   15.00    --   41.77  77.00 120.00  106
 20  \w     15.00 112.00   1.00   15.00    --   41.77  57.00  60.00   97
 21  \w      1.00  82.00   1.00   15.00    --   41.77 -99.00 -90.00   81
 22  \w     10.00 116.00   1.00   15.00    --   41.77  77.00 -60.00  106
 23  \w     10.00  88.00   1.00   15.00    --   41.77  77.00-180.00   78
 24  \w     15.00 112.00   1.00   15.00    --   41.77  57.00-120.00   97
;
_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      0.0075747000
_diffrn_orient_matrix_UB_12      -0.2432064000
_diffrn_orient_matrix_UB_13      -0.0129191000
_diffrn_orient_matrix_UB_21      0.0028205000
_diffrn_orient_matrix_UB_22      -0.0670522000
_diffrn_orient_matrix_UB_23      0.0489935000
_diffrn_orient_matrix_UB_31      -0.0849455000
_diffrn_orient_matrix_UB_32      -0.0237824000
_diffrn_orient_matrix_UB_33      -0.0063113000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            28071
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.683
_diffrn_reflns_theta_min         2.681
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63348
_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    1.389
_exptl_crystal_description       needle
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.029
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.247
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         6938
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0550P)^2^+1.3951P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1270
_refine_ls_wR_factor_ref         0.1408
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5305
_reflns_number_total             6938
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04744d2.cif
_cod_data_source_block           mc184
_cod_depositor_comments
'Adding full bibliography for 7045596--7045600.cif.'
_cod_original_cell_volume        3341.12(17)
_cod_database_code               7045598
_chemical_oxdiff_formula         'C188 H120 N20 O8'
_chemical_oxdiff_usercomment     CF1032
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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.a Aromatic/amide H refined with riding coordinates:
 C2(H2A), 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), N2(H2), C2B(H2B), C3B(H3B),
 C4B(H4B), C5B(H5B), C5BA(H5BA), C7B(H7B), C8B(H8B), C11B(H11B), C13B(H13B),
 C16B(H16B), C18B(H18B), C19B(H19B), C20B(H20B), C21B(H21B)
2.b Idealised tetrahedral OH refined as rotating group:
 O1B(H1B)
;
_shelx_res_checksum              88625
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2017-03-06
_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 1.753
_oxdiff_exptl_absorpt_empirical_full_min 0.483