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_7048201
_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 H40 Ag4 F3 N16 O11 S, 3(C F3 O3 S), 4(C3 H6 O), C3 H7'
_chemical_formula_sum            'C79 H71 Ag4 F12 N16 O24 S4'
_chemical_formula_weight         2416.23
_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             2018-06-27
_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                103.4320(10)
_cell_angle_beta                 93.0640(10)
_cell_angle_gamma                92.0220(10)
_cell_formula_units_Z            2
_cell_length_a                   12.5264(3)
_cell_length_b                   15.3015(4)
_cell_length_c                   25.0246(7)
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.180
_cell_volume                     4653.0(2)
_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      99.98
_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 0.993
_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  0.0340
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_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       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            67838
_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         28.330
_diffrn_reflns_theta_min         1.370
_diffrn_source                   'standard sealed X-ray tube'
_diffrn_source_type              'Siemens, KFF Mo 2K -90 C'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.024
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6408
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0569 before and 0.0438 after correction. The Ratio of minimum to maximum transmission is 0.8593. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2418
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         4.424
_refine_diff_density_min         -2.444
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1398
_refine_ls_number_reflns         23053
_refine_ls_number_restraints     122
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_gt           0.0572
_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^)+(0.0564P)^2^+23.1448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1308
_refine_ls_wR_factor_ref         0.1573
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15257
_reflns_number_total             23053
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04583f2.cif
_cod_data_source_block           hexane4
_cod_depositor_comments
'Adding full bibliography for 7048201--7048212.cif.'
_cod_database_code               7048201
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.853
_shelx_estimated_absorpt_t_min   0.650
_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-F13
 2.6 with sigma of 0.02
 F8-F10
 2.1 with sigma of 0.05
 F7-F11
 2 with sigma of 0.05
 F14-C63 \\sim F15-C63 \\sim F13-C63
 with sigma of 0.02
 S5-O19 \\sim S5-O21 \\sim S5-O20
 with sigma of 0.02
 C72-C71 \\sim C70-C71
 with sigma of 0.02
 C74-C73 \\sim C74-C75
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F7) \\sim Ueq, Uanis(F10) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C73) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O19) = Uanis(O18)
Uanis(O16) = Uanis(F13)
Uanis(F7) = Uanis(F10)
4. Rigid body (RIGU) restrains
 S5, F13, F14, F15, O19, O20, O21, C63
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O15, C70, C71, C72
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O15, C73, C74, C75
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: F7(0.5) F8(0.5) F9(0.5) F10(0.5) F11(0.5) F12(0.5) O10(0.5)
 O11(0.5) O12(0.5) O13(0.5) C61(0.5) C62(0.5) S4(0.75) F16(0.75) F17(0.75)
 F18(0.75) O16(0.75) O17(0.75) O18(0.75) C64(0.75) S5(0.25) F13(0.25) F14(0.25)
 F15(0.25) O19(0.25) O20(0.25) O21(0.25) C63(0.25) C70(0.75) H70A(0.75)
 H70B(0.75) H70C(0.75) C71(0.75) C72(0.75) H72A(0.75) H72B(0.75) H72C(0.75)
 C73(0.25) H73A(0.25) H73B(0.25) H73C(0.25) C74(0.25) C75(0.25) H75A(0.25)
 H75B(0.25) H75C(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C82(H82A,H82B), C83(H83A,H83B)
6.b 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), C17(H17), C19(H19), C20(H20), 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.c Idealised Me refined as rotating group:
 C70(H70A,H70B,H70C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C75(H75A,H75B,
 H75C), C79(H79A,H79B,H79C), C81(H81A,H81B,H81C), C76(H76A,H76B,H76C), C78(H78A,
 H78B,H78C), C67(H67A,H67B,H67C), C69(H69A,H69B,H69C), C84(H84A,H84B,H84C)
;
_shelx_res_checksum              68066
_olex2_submission_special_instructions 'No special instructions were received'