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_7048206
_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 O17.02 S3, C0.83 F2.5 O2.67 S0.83, 2.75(C4 H8 O2), C H2 O0.58'
_chemical_formula_sum            'C75.84 H64 Ag4 F11.5 N16 O25.77 S3.84'
_chemical_formula_weight         2384.70
_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
_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                107.193(2)
_cell_angle_beta                 83.606(3)
_cell_angle_gamma                92.800(2)
_cell_formula_units_Z            2
_cell_length_a                   12.532(3)
_cell_length_b                   15.486(4)
_cell_length_c                   25.142(6)
_cell_measurement_reflns_used    9567
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.698
_cell_measurement_theta_min      2.337
_cell_volume                     4632(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      99.99
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_unetI/netI     0.0570
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            67205
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.739
_diffrn_reflns_theta_min         1.635
_exptl_absorpt_coefficient_mu    1.025
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0897 before and 0.0623 after correction. The Ratio of minimum to maximum transmission is 0.7941. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2380
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.274
_refine_diff_density_min         -2.028
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1392
_refine_ls_number_reflns         19517
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1499
_refine_ls_R_factor_gt           0.0956
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+75.9345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2000
_refine_ls_wR_factor_ref         0.2334
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12609
_reflns_number_total             19517
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04583f2.cif
_cod_data_source_block           dioxane4
_cod_depositor_comments
'Adding full bibliography for 7048201--7048212.cif.'
_cod_original_cell_volume        4631.5(18)
_cod_original_formula_sum        'C75.84 H64 Ag4 F11.50 N16 O25.77 S3.84'
_cod_database_code               7048206
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.845
_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
2. Restrained distances
 C81-C80
 1.3 with sigma of 0.01
 S5-C85
 1.85 with sigma of 0.01
 F14-F15
 2 with sigma of 0.01
 S4-O33 \\sim S4-O31 \\sim S4-O30
 with sigma of 0.02
 F14-C85 \\sim F13-C85 \\sim F15-C85
 with sigma of 0.01
 S1-O14 \\sim S1-O9
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O22 \\sim O21 \\sim C68 \\sim C69 \\sim C70 \\sim C71: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O28) \\sim Ueq, Uanis(C82) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O33) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(F14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(F13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O14) \\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C76) = Uanis(O26)
Uanis(F14) = Uanis(C85)
Uanis(F15) = Uanis(C85)
Uanis(F14) = Uanis(F12)
Uanis(S4) = Uanis(S5)
4. Rigid body (RIGU) restrains
 N9, C31, C32
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O26, C80, C81
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F11, F12, C84
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 S4, F14
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(O13)=1-FVAR(1)
 Sof(O12)=FVAR(1)
 Fixed Sof: O14(0.25) S4(0.33333) F10(0.5) F11(0.5) F12(0.5) F13(0.33333)
 F14(0.33333) F15(0.33333) O29(0.5) S5(0.5) O31(0.33333) O32(0.5) O33(0.33333)
 C84(0.5) C85(0.33333) O23(0.75) O24(0.75) C72(0.75) H72A(0.75) H72B(0.75)
 C73(0.75) H73A(0.75) H73B(0.75) C74(0.75) H74A(0.75) H74B(0.75) C75(0.75)
 H75A(0.75) H75B(0.75) O22(0.5) O21(0.5) C68(0.5) H68A(0.5) H68B(0.5) C69(0.5)
 H69A(0.5) H69B(0.5) C70(0.5) H70A(0.5) H70B(0.5) C71(0.5) H71A(0.5) H71B(0.5)
 O25(0.5) O27(0.5) C77(0.5) H77A(0.5) H77B(0.5) C78(0.5) H78A(0.5) H78B(0.5)
 C79(0.5) H79A(0.5) H79B(0.5) C83(0.5) H83A(0.5) H83B(0.5) O26(0.33333)
 O28(0.25) C76(0.25) H76A(0.25) H76B(0.25) C80(0.25) H80A(0.25) H80B(0.25)
 C81(0.25) H81A(0.25) H81B(0.25) C82(0.25) H82A(0.25) H82B(0.25)
6.a Free rotating group:
 O30(S5), O22(O21,C68,C69,C70,C71)
6.b Secondary CH2 refined with riding coordinates:
 C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B), C72(H72A,
 H72B), C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C68(H68A,H68B),
 C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B), C77(H77A,H77B), C78(H78A,H78B),
  C79(H79A,H79B), C83(H83A,H83B), C76(H76A,H76B), C80(H80A,H80B), C81(H81A,
 H81B), C82(H82A,H82B)
6.c 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), C33(H33),
 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)
;
_shelx_res_checksum              73707
_olex2_submission_special_instructions 'No special instructions were received'