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_7048209
_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
'C61.82 H40 Ag4 F6 N16 O14 S2, 2(C F3 O3 S), 3.25(C4 H8 O)'
_chemical_formula_sum            'C76.82 H66 Ag4 F12 N16 O23.25 S4'
_chemical_formula_weight         2372.95
_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             2018-10-09
_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                104.2650(10)
_cell_angle_beta                 94.1030(10)
_cell_angle_gamma                90.1400(10)
_cell_formula_units_Z            2
_cell_length_a                   12.6763(9)
_cell_length_b                   15.3591(11)
_cell_length_c                   25.2633(18)
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.41
_cell_volume                     4753.8(6)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            61346
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.396
_diffrn_reflns_theta_min         1.415
_exptl_absorpt_coefficient_mu    1.000
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6086
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0602 before and 0.0406 after correction. The Ratio of minimum to maximum transmission is 0.8161. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2370
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.570
_refine_diff_density_min         -2.042
_refine_diff_density_rms         0.163
_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     1492
_refine_ls_number_reflns         23747
_refine_ls_number_restraints     756
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1147
_refine_ls_R_factor_gt           0.0784
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1249P)^2^+26.5528P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2160
_refine_ls_wR_factor_ref         0.2499
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16190
_reflns_number_total             23747
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04583f2.cif
_cod_data_source_block           thf4
_cod_depositor_comments
'Adding full bibliography for 7048201--7048212.cif.'
_cod_database_code               7048209
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.708
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O8-N12 \\sim O6-N13
 with sigma of 0.02
 C46-C45 \\sim C41-C40
 with sigma of 0.02
 C45-C44 \\sim C40-C39
 with sigma of 0.02
 C44-C38 \\sim C39-C43
 with sigma of 0.02
 C44-N12 \\sim C39-N13
 with sigma of 0.02
 C37-C38 \\sim C42-C43
 with sigma of 0.02
 O7-N12 \\sim O5-N13
 with sigma of 0.02
 C33-C46 \\sim C33-C41
 with sigma of 0.04
 C33-C37 \\sim C33-C42
 with sigma of 0.04
 O8-C44 \\sim O6-C39
 with sigma of 0.04
 O8-O7 \\sim O6-O5
 with sigma of 0.04
 C46-C44 \\sim C41-C39
 with sigma of 0.04
 C46-C37 \\sim C41-C42
 with sigma of 0.04
 C45-C38 \\sim C40-C43
 with sigma of 0.04
 C45-N12 \\sim C40-N13
 with sigma of 0.04
 C44-C37 \\sim C39-C42
 with sigma of 0.04
 C44-O7 \\sim C39-O5
 with sigma of 0.04
 C38-N12 \\sim C43-N13
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O32 \\sim C81 \\sim C82 \\sim C83 \\sim C84: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
O31 \\sim C77 \\sim C78 \\sim C79 \\sim C80: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C36 \\sim C37 \\sim C38 \\sim C44 \\sim C45 \\sim C46: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
O5 \\sim O6 \\sim O7 \\sim O8 \\sim N12 \\sim N13 \\sim C36 \\sim C37 \\sim C38
\\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim
C46: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
C16 \\sim H16 \\sim C17 \\sim H17 \\sim S5 \\sim F13 \\sim F15 \\sim O28 \\sim
O29 \\sim O30 \\sim C71 \\sim S6 \\sim F16 \\sim F17 \\sim O25 \\sim O26 \\sim
O27 \\sim C72 \\sim F14 \\sim F18: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C80) \\sim Ueq, Uanis(O31) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C79)
\\sim Ueq, Uanis(C78) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(F14) = Uanis(F16)
Uanis(S2) = Uanis(S3)
Uanis(O19) = Uanis(O22) = Uanis(O20) = Uanis(O24) = Uanis(O21) = Uanis(O23)
Uanis(F19) = Uanis(F1A) = Uanis(F6) = Uanis(F5) = Uanis(F4) = Uanis(F1B)
Uanis(C69) = Uanis(C70)
4. Rigid body (RIGU) restrains
 S6, F16, F17, F18, O25, O26, O27, C72
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 S5, F13, F14, F15, O28, O29, O30, C71
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.002
 O34, C89, C90, C91, C92
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(O31)=Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(C79)=
 Sof(H79A)=Sof(H79B)=Sof(C80)=Sof(H80A)=Sof(H80B)=0.75*(1-FVAR(2))
 Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(O32)=Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(C82)=
 Sof(H82A)=Sof(H82B)=Sof(C83)=Sof(H83A)=Sof(H83B)=0.75*FVAR(2)
 Sof(O5)=Sof(O6)=Sof(N13)=Sof(C39)=Sof(C40)=Sof(H40)=Sof(C41)=Sof(H41)=
 Sof(C42)=Sof(H42)=Sof(C43)=Sof(H43)=1-FVAR(2)
 Sof(O7)=Sof(O8)=Sof(N12)=Sof(C36)=Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38)=
 Sof(C44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=FVAR(2)
 Sof(S3)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(O22)=Sof(O23)=Sof(O24)=Sof(C70)=1-FVAR(3)
 Sof(S2)=Sof(F1B)=Sof(F1A)=Sof(F19)=Sof(O19)=Sof(O20)=Sof(O21)=Sof(C69)=FVAR(3)
 Fixed Sof: F7(0.5) F8(0.5) F9(0.5) F10(0.5) F11(0.5) F12(0.5) O15(0.5)
 O16(0.5) O17(0.5) O18(0.5) C67(0.5) C68(0.5) S5(0.4) F13(0.4) F14(0.4)
 F15(0.4) O28(0.4) O29(0.4) O30(0.4) C71(0.4) S6(0.6) F16(0.6) F17(0.6)
 F18(0.6) O25(0.6) O26(0.6) O27(0.6) C72(0.6) C93(0.5) H93A(0.5) H93B(0.5)
 C94(0.5) H94A(0.5) H94B(0.5) C95(0.5) H95A(0.5) H95B(0.5) C96(0.5) H96A(0.5)
 H96B(0.5) C97(0.5) H97A(0.5) H97B(0.5) C98(0.5) H98A(0.5) H98B(0.5) C99(0.5)
 H99A(0.5) H99B(0.5) C100(0.5) H10A(0.5) H10B(0.5) O36(0.5) C73(0.5) H73A(0.5)
 H73B(0.5) C74(0.5) H74A(0.5) H74B(0.5) C75(0.5) H75A(0.5) H75B(0.5) C76(0.5)
 H76A(0.5) H76B(0.5) O34(0.5) C89(0.5) H89A(0.5) H89B(0.5) C90(0.5) H90A(0.5)
 H90B(0.5) C91(0.5) H91A(0.5) H91B(0.5) C92(0.5) H92A(0.5) H92B(0.5) O33(0.5)
 C85(0.5) H85A(0.5) H85B(0.5) C86(0.5) H86A(0.5) H86B(0.5) C87(0.5) H87A(0.5)
 H87B(0.5) C88(0.5) H88A(0.5) H88B(0.5)
6.a Free rotating group:
 S3(F4,F5,F6,O22,O23,O24,C70), S5(F13,F14,F15,O28,O29,O30,C71), S2(F1B,F1A,F19,
 O19,O20,O21,C69), S6(F16,F17,F18,O25,O26,O27,C72), C84(O32,C81,C82,C83),
 O31(C77,C78,C79,C80)
6.b Secondary CH2 refined with riding coordinates:
 C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B), C96(H96A,H96B), C97(H97A,
 H97B), C98(H98A,H98B), C99(H99A,H99B), C100(H10A,H10B), C73(H73A,H73B),
 C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C89(H89A,H89B), C90(H90A,H90B),
  C91(H91A,H91B), C92(H92A,H92B), C84(H84A,H84B), C81(H81A,H81B), C82(H82A,
 H82B), C83(H83A,H83B), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B),
 C88(H88A,H88B), C77(H77A,H77B), C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C22(H22), C23(H23), C25(H25),
  C26(H26), C28(H28), C29(H29), C30(H30), C32(H32), C34(H34), C35(H35),
 C37(H37), C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C45(H45), C46(H46),
  C47(H47), C49(H49), C50(H50), C51(H51), C52(H52), C54(H54), C57(H57),
 C58(H58), C60(H60), C61(H61), C63(H63), C64(H64), C65(H65)
;
_shelx_res_checksum              89249
_olex2_submission_special_instructions 'No special instructions were received'