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_7048202
_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
'C62 H40 Ag4 F6 N16 O14 S2, 2(C F3 O3 S), 1.33(C7 H8), C2.67 H5 O, 0.75(C3 H6 O)'
_chemical_formula_sum            'C78.25 H60.17 Ag4 F12 N16 O21.75 S4'
_chemical_formula_weight         2360.31
_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             2018-10-10
_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                104.421(2)
_cell_angle_beta                 90.943(2)
_cell_angle_gamma                91.173(2)
_cell_formula_units_Z            2
_cell_length_a                   12.1193(13)
_cell_length_b                   15.7806(17)
_cell_length_c                   24.659(3)
_cell_measurement_reflns_used    8873
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.28
_cell_measurement_theta_min      2.33
_cell_volume                     4565.3(9)
_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      100.02
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_unetI/netI     0.0686
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            69092
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.504
_diffrn_reflns_theta_min         1.333
_exptl_absorpt_coefficient_mu    1.040
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_description       block
_exptl_crystal_F_000             2351
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.621
_refine_diff_density_min         -1.332
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1379
_refine_ls_number_reflns         16601
_refine_ls_number_restraints     563
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.0606
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1091P)^2^+11.8966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1665
_refine_ls_wR_factor_ref         0.2020
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10095
_reflns_number_total             16601
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04583f2.cif
_cod_data_source_block           PhMe4
_cod_depositor_comments
'Adding full bibliography for 7048201--7048212.cif.'
_cod_original_cell_volume        4565.4(8)
_cod_database_code               7048202
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.598
_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
 C80-C85 = C75-C74
 1.5 with sigma of 0.02
 C86-C87
 1.5 with sigma of 0.02
 C78-C85
 2.48 with sigma of 0.04
 C81-C85
 2.48 with sigma of 0.04
 C86-C93
 2.48 with sigma of 0.04
 C86-C88
 2.48 with sigma of 0.04
3. Restrained planarity
 C72, C73, C77, C78, C80, C81, C85
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(S5) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O20) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.01
Uanis(C90) \\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(C87)
\\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C93) \\sim Ueq, Uanis(C86) \\sim Ueq:
with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C74) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C73)
\\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C81) \\sim Ueq,
Uanis(C83) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C75)
\\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C85) \\sim Ueq:
with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C95) \\sim Ueq, Uanis(C97) \\sim Ueq, Uanis(C98) \\sim Ueq, Uanis(C96)
\\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C99) \\sim Ueq, Uanis(C94) \\sim Ueq:
with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(S4) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O23)
\\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F13) \\sim Ueq,
Uanis(F12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C84) = Uanis(C85)
Uanis(C91) = Uanis(C92)
Uanis(C87) = Uanis(C96)
Uanis(C97) = Uanis(C87)
5. Rigid body (RIGU) restrains
 S4, F11, F12, F13, O21, O22, O23, C64
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 S5, F10, F14, F15, O18, O19, O20, C63
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Fixed Sof: S5(0.5) F10(0.5) F14(0.5) F15(0.5) O18(0.5) O19(0.5) O20(0.5)
 C63(0.5) S4(0.5) F11(0.5) F12(0.5) F13(0.5) O21(0.5) O22(0.5) O23(0.5)
 C64(0.5) C97(0.3) H97(0.3) C98(0.3) C91(0.3) H91(0.3) C95(0.3) H95(0.3)
 C94(0.3) H94(0.3) C96(0.3) H96(0.3) C99(0.3) H99a(0.3) H99b(0.3) H99c(0.3)
 C86(0.2) H86a(0.2) H86b(0.2) H86c(0.2) C89(0.2) H89(0.2) C88(0.2) H88(0.2)
 C87(0.2) C93(0.2) H93(0.2) C92(0.2) H92(0.2) C90(0.2) H90(0.2) C74(0.5)
 H74a(0.5) H74b(0.5) H74c(0.5) C83(0.5) H83(0.5) C84(0.5) H84(0.5) C79(0.5)
 H79(0.5) C75(0.5) C76(0.5) H76(0.5) C82(0.5) H82(0.5) C80(0.33333)
 C78(0.33333) H78(0.33333) C73(0.33333) H73(0.33333) C72(0.33333) H72(0.33333)
 C77(0.33333) H77(0.33333) C81(0.33333) H81(0.33333) C85(0.33333) H85a(0.33333)
 H85b(0.33333) H85c(0.33333) C68(0.667) H68a(0.667) H68b(0.667) H68c(0.667)
 O25(0.75) C69(0.75) H69a(0.75) H69b(0.75) H69c(0.75) C70(0.75) C71(0.75)
 H71a(0.75) H71b(0.75) H71c(0.75)
7.a Free rotating group:
 S5(F10,F14,F15,O18,O19,O20,C63), S4(F11,F12,F13,O21,O22,O23,C64)
7.b Me refined with riding coordinates:
 C99(H99a,H99b,H99c), C86(H86a,H86b,H86c), C74(H74a,H74b,H74c), C85(H85a,H85b,
 H85c)
7.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), 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), C31(H31), C32(H32), C34(H34),
 C37(H37), C38(H38), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45), C47(H47),
  C49(H49), C50(H50), C52(H52), C53(H53), C55(H55), C56(H56), C58(H58),
 C59(H59), C60(H60), C97(H97), C91(H91), C95(H95), C94(H94), C96(H96), C89(H89),
  C88(H88), C93(H93), C92(H92), C90(H90), C83(H83), C84(H84), C79(H79),
 C76(H76), C82(H82), C78(H78), C73(H73), C72(H72), C77(H77), C81(H81)
7.d Fitted hexagon refined as free rotating group:
 C97(C98,C91,C95,C94,C96), C89(C88,C87,C93,C92,C90), C83(C84,C79,C75,C76,C82),
 C80(C78,C73,C72,C77,C81)
7.e Idealised Me refined as rotating group:
 C66(H66a,H66b,H66c), C68(H68a,H68b,H68c), C69(H69a,H69b,H69c), C71(H71a,H71b,
 H71c)
;
_shelx_res_checksum              36784
_olex2_submission_special_instructions 'No special instructions were received'