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_7048203
_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
'C63 H40 Ag4 F9 N16 O17 S3, C Cl4, C F3 O3 S, 4(C3 H6 O)'
_chemical_formula_sum            'C77 H60 Ag4 Cl4 F12 N16 O24 S4'
_chemical_formula_weight         2522.93
_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                103.3030(10)
_cell_angle_beta                 93.6400(10)
_cell_angle_gamma                93.3890(10)
_cell_formula_units_Z            2
_cell_length_a                   12.5434(4)
_cell_length_b                   15.3059(5)
_cell_length_c                   25.2934(8)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.23
_cell_volume                     4702.6(3)
_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      99.93
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 area detector'
_diffrn_measurement_method       '\w and \f 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  0.0322
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            66530
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.394
_diffrn_reflns_theta_min         1.426
_diffrn_source                   'standard sealed X-ray tube'
_diffrn_source_type              'Siemens, KFF Mo 2K -90 C'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.128
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0502 before and 0.0396 after correction. The Ratio of minimum to maximum transmission is 0.8914. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2508
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.774
_refine_diff_density_min         -2.414
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1431
_refine_ls_number_reflns         23507
_refine_ls_number_restraints     236
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0742P)^2^+26.4210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1641
_refine_ls_wR_factor_ref         0.1849
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16695
_reflns_number_total             23507
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04583f2.cif
_cod_data_source_block           ccl44
_cod_depositor_comments
'Adding full bibliography for 7048201--7048212.cif.'
_cod_database_code               7048203
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.781
_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 Cl(H,H) groups
2. Restrained distances
 F2-F3
 2 with sigma of 0.01
 S2-O19
 1.4 with sigma of 0.02
 C16-H16
 0.95 with sigma of 0.01
 C31-H31
 0.95 with sigma of 0.01
 C72-C73 \\sim C74-C73
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C67) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O25) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(F12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C74) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(F4) = Uanis(F3)
Uanis(C73) = Uanis(C70)
Uanis(O28) = Uanis(O23)
Uanis(C69) = Uanis(C74)
Uanis(Cl3B) = Uanis(Cl2B) = Uanis(Cl4B) = Uanis(Cl1A) = Uanis(Cl3A) =
Uanis(Cl2A) = Uanis(Cl4A)
4. Rigid body (RIGU) restrains
 F1, F2, F3, C61
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 S4, F14, F17, F18, O23, O24, O25, C67
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 S6, F10, F11, F12, O26, O27, O28, C68
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C69, C70, C71
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C72, C73, C74
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 S5, F13, F15, F16, O20, O21, O22, C66
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(Cl2B)=Sof(Cl3B)=Sof(Cl4B)=1-FVAR(1)
 Sof(Cl2A)=Sof(Cl3A)=Sof(Cl4A)=FVAR(1)
 Fixed Sof: F1(0.33333) F2(0.33333) F3(0.33333) F4(0.6667) F5(0.6667)
 F6(0.6667) O10(0.33333) O11(0.6667) O12(0.6667) O13(0.33333) C61(0.33333)
 C62(0.6667) S6(0.25) F10(0.25) F11(0.25) F12(0.25) O26(0.25) O27(0.25)
 O28(0.25) C68(0.25) S4(0.25) F14(0.25) F17(0.25) F18(0.25) O23(0.25) O24(0.25)
 O25(0.25) C67(0.25) S5(0.5) F13(0.5) F15(0.5) F16(0.5) O20(0.5) O21(0.5)
 O22(0.5) C66(0.5) C69(0.6667) H69A(0.6667) H69B(0.6667) H69C(0.6667)
 C70(0.6667) C71(0.6667) H71A(0.6667) H71B(0.6667) H71C(0.6667) C72(0.33333)
 H72A(0.33333) H72B(0.33333) H72C(0.33333) C73(0.33333) C74(0.33333)
 H74A(0.33333) H74B(0.33333) H74C(0.33333)
6.a Free rotating group:
 S6(F10,F11,F12,O26,O27,O28,C68), S4(F14,F17,F18,O23,O24,O25,C67), S5(F13,F15,
 F16,O20,O21,O22,C66)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C12(H12), C14(H14), C15(H15),
 C17(H17), C19(H19), C22(H22), C23(H23), C25(H25), C26(H26), C28(H28), C29(H29),
  C30(H30), C32(H32), C34(H34), 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.c Idealised Me refined as rotating group:
 C69(H69A,H69B,H69C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C74(H74A,H74B,
 H74C), C78(H78A,H78B,H78C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C), C83(H83A,
 H83B,H83C), C75(H75A,H75B,H75C), C77(H77A,H77B,H77C)
;
_shelx_res_checksum              74598
_olex2_submission_special_instructions 'No special instructions were received'