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_7048205
_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), 2.5(C4 H8 O2), C3 H6.5 O1.5'
_chemical_formula_sum            'C77.34 H65.67 Ag4 F12 N16 O26.33 S4'
_chemical_formula_weight         2428.22
_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             2018-10-09
_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                102.9490(10)
_cell_angle_beta                 92.2200(10)
_cell_angle_gamma                94.3740(10)
_cell_formula_units_Z            2
_cell_length_a                   12.5618(11)
_cell_length_b                   15.2290(13)
_cell_length_c                   24.842(2)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.223
_cell_volume                     4610.4(7)
_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      99.99
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0754
_diffrn_reflns_av_unetI/netI     0.0928
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            69623
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.308
_diffrn_reflns_theta_min         1.441
_diffrn_source                   'standard sealed X-ray tube'
_diffrn_source_type              'Siemens, KFF Mo 2K -90 C'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.036
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5360
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0826 before and 0.0579 after correction. The Ratio of minimum to maximum transmission is 0.7188. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2425
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.487
_refine_diff_density_min         -1.321
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1430
_refine_ls_number_reflns         22892
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1377
_refine_ls_R_factor_gt           0.0583
_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^)+(0.0974P)^2^+3.7723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1465
_refine_ls_wR_factor_ref         0.1934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12157
_reflns_number_total             22892
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04583f2.cif
_cod_data_source_block           EtOAc4
_cod_depositor_comments
'Adding full bibliography for 7048201--7048212.cif.'
_cod_original_cell_volume        4610.5(7)
_cod_database_code               7048205
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.746
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S5-O17 \\sim S5-O16 \\sim S5-O18
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O29 \\sim C74 \\sim C75: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C62) \\sim Ueq: with sigma of 0.2 and sigma for terminal atoms of 0.2
Uanis(O23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C74) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(O29) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 S5, O16, O17, O18
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: S2(0.667) S3(0.33333) F4(0.667) F5(0.667) F6(0.667) F7(0.33333)
 F8(0.33333) F9(0.33) O13(0.667) O15(0.33333) C62(0.33333) C63(0.667)
 S5(0.33333) F13(0.33333) F14(0.33333) F15(0.33333) O16(0.33333) O17(0.33333)
 O18(0.33333) C65(0.33333) S6(0.667) F16(0.667) F17(0.667) F18(0.667)
 O19(0.667) O20(0.667) O21(0.667) C66(0.667) O29(0.75) O30(0.75) C74(0.75)
 H74A(0.75) H74B(0.75) H74C(0.75) C75(0.75) C76(0.75) C77(0.75) H77A(0.75)
 H77B(0.75) H77C(0.75) O27(0.5) O28(0.5) C70(0.5) C71(0.5) H71A(0.5) H71B(0.5)
 H71C(0.5) C72(0.5) H72A(0.5) H72B(0.5) H72C(0.5) C73(0.5) H73A(0.5) H73B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C68(H68A,H68B), C75(H75A,H75B), C79(H79A,H79B), C73(H73A,H73B)
6.b Me refined with riding coordinates:
 C77(H77A,H77B,H77C)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 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), 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:
 C67(H67A,H67B,H67C), C69(H69A,H69B,H69C), C74(H74A,H74B,H74C), C78(H78A,H78B,
 H78C), C81(H81A,H81B,H81C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C)
;
_shelx_res_checksum              88930
_olex2_submission_special_instructions 'No special instructions were received'