Exploring the reversible host-guest chemistry of a crystalline octanuclear Ag(i) metallosupramolecular macrocycle formed from a simple pyrazinylpyridine ligand.
Dalton, Hannah L.; Lynes, Amy D.; Twamley, Brendan; Byrne, Kevin; Schmitt, Wolfgang; Hawes, Chris S.; Gunnlaugsson, Thorfinnur; Dalton transactions (Cambridge, England : 2003) 47 (2018) 17266–17275; doi:10.1039/c8dt04583f

data_7048207
_publ_section_title
;
 Exploring the reversible host-guest chemistry of a crystalline
 octanuclear Ag(i) metallosupramolecular macrocycle formed from a simple
 pyrazinylpyridine ligand.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17266
_journal_page_last               17275
_journal_paper_doi               10.1039/c8dt04583f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'C61 H40 Ag4 F3 N16 O11 S, 2(C F3 O3 S), 2.33(C2.25 H4.5 O0.75), 1.71(C6 H6), C F2.75 O3 S'
_chemical_formula_sum            'C79.5 H60.75 Ag4 F11.75 N16 O21.75 S4'
_chemical_formula_weight         2371.16
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-10 deposited with the CCDC.
2018-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                104.5980(10)
_cell_angle_beta                 88.806(2)
_cell_angle_gamma                90.245(2)
_cell_formula_units_Z            2
_cell_length_a                   12.1199(6)
_cell_length_b                   15.9796(7)
_cell_length_c                   24.4413(11)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.402
_cell_measurement_theta_min      2.410
_cell_volume                     4579.8(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX 3 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1388
_diffrn_reflns_av_unetI/netI     0.1558
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            67105
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.403
_diffrn_reflns_theta_min         1.380
_diffrn_source                   'standard sealed X-ray tube'
_diffrn_source_type              'Siemens, KFF Mo 2K -90 C'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.037
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1022 before and 0.0790 after correction. The Ratio of minimum to maximum transmission is 0.7473. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2363
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.833
_refine_diff_density_min         -1.204
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1297
_refine_ls_number_reflns         16628
_refine_ls_number_restraints     214
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1847
_refine_ls_R_factor_gt           0.0820
_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^)+(0.1063P)^2^+0.0681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1789
_refine_ls_wR_factor_ref         0.2198
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7819
_reflns_number_total             16628
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04583f2.cif
_cod_data_source_block           benzene4
_cod_depositor_comments
'Adding full bibliography for 7048201--7048212.cif.'
_cod_original_formula_sum        'C79.50 H60.75 Ag4 F11.75 N16 O21.75 S4'
_cod_database_code               7048207
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.819
_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
2. Restrained distances
 C0AA-F10
 1.5 with sigma of 0.01
 S4-C0AA
 1.8 with sigma of 0.01
 S4-O1A
 1.5 with sigma of 0.01
 C0AA-F12
 1.5 with sigma of 0.01
 C1AA-F23
 1.5 with sigma of 0.01
 C1AA-S0AA
 1.8 with sigma of 0.01
 C1AA-F14
 1.5 with sigma of 0.01
 C79-C78 = C65-C70
 1.39 with sigma of 0.01
 F10-C0AA \\sim F11-C0AA \\sim F12-C0AA
 with sigma of 0.01
 F23-C1AA \\sim F1AA-C1AA
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C75 \\sim C76 \\sim C71 \\sim C74 \\sim C72 \\sim C73: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
C80 \\sim C81 \\sim C82 \\sim C77 \\sim C79 \\sim C78: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C74 \\sim C73 \\sim C72: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C80 \\sim C79 \\sim C78: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C82 \\sim C81 \\sim C77 \\sim C78: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
O1A \\sim S4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
F12 \\sim C0AA \\sim F11: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O1AA \\sim S0AA \\sim O19: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
F1AA \\sim C1AA \\sim F23 \\sim F14: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C87) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C81) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F11) \\sim Ueq, Uanis(S4) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O1A)
\\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F12) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.02
Uanis(F23) \\sim Ueq, Uanis(F1AA) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C1AA) \\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F1AA) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(C89) = Uanis(C88)
Uanis(C77) = Uanis(C82)
Uanis(C78) = Uanis(C76)
Uanis(C88) = Uanis(C86)
Uanis(C89) = Uanis(C86)
Uanis(F10) = Uanis(C0AA)
Uanis(F23) = Uanis(C1AA)
Uanis(C0AA) = Uanis(C1AA)
Uanis(F14) = Uanis(C1AA)
4. Rigid body (RIGU) restrains
 C88, C86, C90
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: O22(0.75) C86(0.75) C90(0.5) H90A(0.5) H90B(0.5) H90C(0.5)
 C76(0.5) H76(0.5) C75(0.5) H75(0.5) C74(0.25) H74(0.25) C73(0.5) H73(0.5)
 C72(0.5) H72(0.5) C71(0.5) H71(0.5) C88(0.5) H88A(0.5) H88B(0.5) H88C(0.5)
 C89(0.25) H89A(0.25) H89B(0.25) H89C(0.25) C87(0.25) H87A(0.25) H87B(0.25)
 H87C(0.25) C80(0.25) H80(0.25) C81(0.25) H81(0.25) C82(0.25) H82(0.25)
 C77(0.25) H77(0.25) C78(0.25) H78(0.25) C79(0.25) H79(0.25) S4(0.5) O1A(0.5)
 F10(0.5) F11(0.5) F12(0.5) C0AA(0.5) S0AA(0.5) O1AA(0.5) C1AA(0.5) F1AA(0.5)
 F23(0.5) F14(0.25)
6.a Free rotating group:
 S4(O19,O1A,F10,F11,F12)
6.b Aromatic/amide H refined with riding coordinates:
 C34(H34), C58(H58), C49(H49), C4(H4), C27(H27), C47(H47), C41(H41), C2(H2),
 C43(H43), C8(H8), C1(H1), C32(H32), C17(H17), C14(H14), C20(H20), C11(H11),
 C53(H53), C7(H7), C31(H31), C22(H22), C60(H60), C30(H30), C25(H25), C15(H15),
 C26(H26), C23(H23), C13(H13), C45(H45), C10(H10), C52(H52), C56(H56), C29(H29),
  C46(H46), C59(H59), C55(H55), C19(H19), C38(H38), C37(H37), C40(H40),
 C44(H44), C66(H66), C67(H67), C69(H69), C68(H68), C70(H70), C65(H65), C76(H76),
  C75(H75), C74(H74), C73(H73), C72(H72), C71(H71), C80(H80), C81(H81),
 C82(H82), C77(H77), C78(H78), C79(H79)
6.c Fitted hexagon refined as free rotating group:
 C66(C67,C69,C68,C70,C65), C76(C75,C74,C73,C72,C71), C80(C81,C82,C77,C78,C79)
6.d Idealised Me refined as rotating group:
 C83(H83A,H83B,H83C), C90(H90A,H90B,H90C), C88(H88A,H88B,H88C), C85(H85A,H85B,
 H85C), C89(H89A,H89B,H89C), C87(H87A,H87B,H87C)
;
_shelx_res_checksum              9274
_olex2_submission_special_instructions 'No special instructions were received'