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_7048212
_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 H41 Ag4 F3 N16 O11.5 S, 3(C F3 O3 S), C2.51 H5.02 O, 3.5(C3 H6 O)'
_chemical_formula_sum            'C77.01 H67.02 Ag4 F12 N16 O25 S4'
_chemical_formula_weight         2404.32
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-27
_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                103.550(4)
_cell_angle_beta                 93.043(6)
_cell_angle_gamma                92.900(7)
_cell_formula_units_Z            2
_cell_length_a                   12.499(2)
_cell_length_b                   15.145(3)
_cell_length_c                   25.237(5)
_cell_measurement_reflns_used    1982
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.66
_cell_measurement_theta_min      2.99
_cell_volume                     4628.0(15)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX 3 (Bruker, 2017) '
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_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(2)
_diffrn_detector                 'CMOS area detector'
_diffrn_detector_area_resol_mean 5.12
_diffrn_detector_type            'Bruker PHOTON 50'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest ECO'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.5 mm double-pinhole'
_diffrn_radiation_detector       'Bruker PHOTON 50'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1595
_diffrn_reflns_av_unetI/netI     0.0824
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            96627
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.481
_diffrn_reflns_theta_min         2.406
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Siemens, KFF Mo 2K -90 C'
_exptl_absorpt_coefficient_mu    1.030
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6306
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0733 before and 0.0604 after correction. The Ratio of minimum to maximum transmission is 0.8462. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2402
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.955
_refine_diff_density_min         -1.079
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1340
_refine_ls_number_reflns         17077
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1364
_refine_ls_R_factor_gt           0.0746
_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^)+(0.1510P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1969
_refine_ls_wR_factor_ref         0.2478
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9514
_reflns_number_total             17077
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04583f2.cif
_cod_data_source_block           acetonediox4
_cod_depositor_comments
'Adding full bibliography for 7048201--7048212.cif.'
_cod_original_cell_volume        4627.9(16)
_cod_database_code               7048212
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.643
_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,H) groups
2. Restrained distances
 S1-C61
 1.8 with sigma of 0.02
 O9-O27
 3.2 with sigma of 0.1
 C63-F16
 1.33 with sigma of 0.01
 F5-C62 \\sim F6-C62 \\sim F4-C62
 with sigma of 0.02
 F3-C61 \\sim F1-C61 \\sim F2-C61
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F17 \\sim F18 \\sim C64: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O19 \\sim O20: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C78) \\sim Ueq, Uanis(O31) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C77)
\\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C81) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C62) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F1) \\sim
Ueq, Uanis(F6) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(O13) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(F8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O27) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C75)
\\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(F16) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F14) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C81) = Uanis(C80)
Uanis(C77) = Uanis(C76)
Uanis(F4) = Uanis(F3)
Uanis(C79) = Uanis(C78)
Uanis(C75) = Uanis(C74) = Uanis(C73) = Uanis(O27)
Uanis(C63) = Uanis(C64)
Uanis(S5) = Uanis(S4)
4. Rigid body (RIGU) restrains
 C77, C78
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 S1, F2, C61
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F5, F6, C62
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F8, F9, C65
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F7, C65
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(S4)=Sof(F13)=Sof(F14)=Sof(F16)=Sof(O18)=Sof(O19)=Sof(O21)=Sof(C63)=1-
 FVAR(1)
 Sof(S5)=Sof(F15)=Sof(F17)=Sof(F18)=Sof(O20)=Sof(O22)=Sof(O23)=Sof(C64)=FVAR(1)
 Fixed Sof: F1(0.5) F2(0.5) F3(0.5) F4(0.5) F5(0.5) F6(0.5) O9(0.5) H9A(0.5)
 H9B(0.5) O11(0.5) O12(0.5) O13(0.5) O14(0.5) C61(0.5) C62(0.5) C76(0.5)
 H76A(0.5) H76B(0.5) H76C(0.5) C77(0.5) C78(0.5) H78A(0.5) H78B(0.5) H78C(0.5)
 C79(0.337) H79A(0.337) H79B(0.337) H79C(0.337) C80(0.337) C81(0.337)
 H81A(0.337) H81B(0.337) H81C(0.337) O27(0.5) C73(0.5) H73A(0.5) H73B(0.5)
 H73C(0.5) C74(0.5) C75(0.5) H75A(0.5) H75B(0.5) H75C(0.5)
6.a Riding coordinates:
 O9(H9A,H9B)
6.b Free rotating group:
 S4(F13,F14,F16,O18,O19,O21,C63), S5(F15,F17,F18,O20,O22,O23,C64), O27(C73,C74,
 C75)
6.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), C17(H17), C19(H19), C20(H20), 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), C43(H43), C44(H44), C45(H45), C46(H46),
  C47(H47), C49(H49), C52(H52), C53(H53), C55(H55), C56(H56), C58(H58),
 C59(H59), C60(H60)
6.d Idealised Me refined as rotating group:
 C76(H76A,H76B,H76C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C81(H81A,H81B,
 H81C), C73(H73A,H73B,H73C), C75(H75A,H75B,H75C), C82(H82A,H82B,H82C), C84(H84A,
 H84B,H84C), C67(H67A,H67B,H67C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C),
 C72(H72A,H72B,H72C)
;
_shelx_res_checksum              12817
_olex2_submission_original_sample_id HLD079_2_114_2_Ace_DIOX_Ace
_olex2_submission_special_instructions 'No special instructions were received'