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_7048204
_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 H41.5 Ag4 F3 N16 O11.75 S, 3(C F3 O3 S), 5(C3 H6 O)'
_chemical_formula_sum            'C79 H71.5 Ag4 F12 N16 O25.75 S4'
_chemical_formula_weight         2444.74
_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     direct
_audit_creation_date             2018-07-02
_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                103.2190(10)
_cell_angle_beta                 93.3530(10)
_cell_angle_gamma                92.5540(10)
_cell_formula_units_Z            2
_cell_length_a                   12.5643(4)
_cell_length_b                   15.0925(5)
_cell_length_c                   25.2576(8)
_cell_measurement_reflns_used    9359
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.523
_cell_measurement_theta_min      2.41
_cell_volume                     4646.3(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    'SIR2004 (Burla et al.,  2007)'
_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 1.000
_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  0.0375
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            117829
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.600
_diffrn_reflns_theta_min         1.388
_diffrn_source                   'standard sealed X-ray tube'
_diffrn_source_type              'Siemens, KFF Mo 2K -90 C'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.028
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0615 before and 0.0443 after correction. The Ratio of minimum to maximum transmission is 0.8378. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2447
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.961
_refine_diff_density_min         -1.035
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1448
_refine_ls_number_reflns         28499
_refine_ls_number_restraints     231
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0470P)^2^+8.5990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1177
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20907
_reflns_number_total             28499
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04583f2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7048201--7048212.cif.'
_cod_original_formula_sum        'C79 H71.50 Ag4 F12 N16 O25.75 S4'
_cod_database_code               7048204
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.708
_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 C(H,H,H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 F12-C84 \\sim F10-C84 \\sim F11-C84
 with sigma of 0.01
 S3-O19 \\sim S3-O18 \\sim S3-O20
 with sigma of 0.01
 S3-C84 \\sim S2-C85
 with sigma of 0.01
 S1-C62 \\sim S1-C61
 with sigma of 0.01
 F6-C61 \\sim F4-C61 \\sim F3-C62 \\sim F1-C62 \\sim F2-C62 \\sim F5-C61
 with sigma of 0.01
 C73-C72 \\sim C73-C74 \\sim C71-C70 \\sim C69-C70
 with sigma of 0.01
 O31-C76 \\sim O30-C77
 with sigma of 0.02
 C76-C75 \\sim C76-C78 \\sim C78-C77 \\sim C75-C77
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 S2, F7, F8, F9, C85
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 S3, F10, F11, F12, O18, C84
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 S1, F1, F2, F3, C62
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 S1, F4, F5, F6, C61
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O29, C69, C70, C71
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O29, C72, C73, C74
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O31, C75, C76, C78
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O30, C75, C77, C78
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Fixed Sof: F1(0.6) F2(0.6) F3(0.6) F4(0.4) F5(0.4) F6(0.4) O2(0.75) H2a(0.75)
 H2b(0.75) O11(0.4) O12(0.4) O13(0.6) O14(0.6) C61(0.4) C62(0.6) S3(0.25)
 F10(0.25) F11(0.25) F12(0.25) O18(0.25) O19(0.25) O20(0.25) C84(0.25) S2(0.75)
 F7(0.75) F8(0.75) F9(0.75) O15(0.75) O16(0.75) O17(0.75) C85(0.75) C69(0.6)
 H69a(0.6) H69b(0.6) H69c(0.6) C70(0.6) C71(0.6) H71a(0.6) H71b(0.6) H71c(0.6)
 C72(0.4) H72a(0.4) H72b(0.4) H72c(0.4) C73(0.4) C74(0.4) H74a(0.4) H74b(0.4)
 H74c(0.4) O30(0.75) O31(0.25) H75a(0.75) H75b(0.75) H75c(0.75) H75d(0.25)
 H75e(0.25) H75f(0.25) C76(0.25) C77(0.75) H78a(0.75) H78b(0.75) H78c(0.75)
 H78d(0.25) H78e(0.25) H78f(0.25)
5.a Rotating group:
 O2(H2a,H2b)
5.b Me refined with riding coordinates:
 C69(H69a,H69b,H69c), C71(H71a,H71b,H71c), C72(H72a,H72b,H72c), C74(H74a,H74b,
 H74c), C75(H75a,H75b,H75c), C75(H75d,H75e,H75f), C78(H78a,H78b,H78c), C78(H78d,
 H78e,H78f)
5.c Me refined as rotating group:
 C66(H66a,H66b,H66c)
5.d 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), 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), C54(H54), C56(H56), C57(H57),
 C59(H59), C60(H60)
5.e Idealised Me refined as rotating group:
 C68(H68a,H68b,H68c), C63(H63a,H63b,H63c), C65(H65a,H65b,H65c), C80(H80a,H80b,
 H80c), C82(H82a,H82b,H82c)
;
_shelx_res_checksum              86540
_olex2_submission_special_instructions 'No special instructions were received'