Synthesis of stable polymetalated aromatic complexes through metal-macrocycle capsule-triggered cyclization.
He, Xin; Xue, Yang; Li, Cui-Cui; Wang, Yuechao; Jiang, Hong; Zhao, Liang; Chemical science 9 (2018) 1481–1487; doi:10.1039/c7sc04503d

data_1548385
_publ_section_title
;
 Synthesis of stable polymetalated aromatic complexes through
 metal-macrocycle capsule-triggered cyclization.
;
_journal_issue                   6
_journal_name_full               'Chemical science'
_journal_page_first              1481
_journal_page_last               1487
_journal_paper_doi               10.1039/c7sc04503d
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C64 H57 Ag5 N17, 3(C F3 O3 S)'
_chemical_formula_sum            'C67 H57 Ag5 F9 N17 O9 S3'
_chemical_formula_weight         2050.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-02-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-06-28 deposited with the CCDC.
2017-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 125.685(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3943(4)
_cell_length_b                   31.0527(14)
_cell_length_c                   22.6971(8)
_cell_measurement_reflns_used    9576
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      71.2270
_cell_measurement_theta_min      4.2300
_cell_volume                     8240.3(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.00(10)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'four-circle diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.2739
_diffrn_reflns_av_unetI/netI     0.1910
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33285
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.475
_diffrn_reflns_theta_min         3.722
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    10.783
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6524
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Pale-yellow
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_description       Plate
_exptl_crystal_F_000             4056
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         7.591
_refine_diff_density_min         -4.412
_refine_diff_density_rms         0.652
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1143
_refine_ls_number_reflns         15612
_refine_ls_number_restraints     319
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.2674
_refine_ls_R_factor_gt           0.2130
_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^)+(0.4000P)^2^+200.0000P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5017
_refine_ls_wR_factor_ref         0.5615
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9503
_reflns_number_total             15612
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc04503d2.cif
_cod_data_source_block           y_sq_s
_cod_depositor_comments
'Adding full bibliography for 1548380--1548386.cif.'
_cod_database_code               1548385
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C67'-F7' = C67'-F8' = C67'-F9'
 1.35 with sigma of 0.01
 F7'-F8' = F7'-F9' = F8'-F9'
 2.15 with sigma of 0.01
 O7'-C67' = O8'-C67' = O9'-C67'
 2.6 with sigma of 0.01
 S3'-F7' = S3'-F8' = S3'-F9'
 2.6 with sigma of 0.01
 C67-F7 = C67-F8 = C67-F9
 1.35 with sigma of 0.01
 F7-F8 = F7-F9 = F8-F9
 2.15 with sigma of 0.01
 S3'-C67'
 1.8 with sigma of 0.02
 C67'-F7' \\sim C67'-F8' \\sim C67'-F9'
 with sigma of 0.02
 F7'-F8' \\sim F7'-F9' \\sim F8'-F9'
 with sigma of 0.02
 S3'-O7' \\sim S3'-O8' \\sim S3'-O9'
 with sigma of 0.02
 O7'-O8' \\sim O7'-O9' \\sim O8'-O9'
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6)
\\sim Ueq, Uanis(C7') \\sim Ueq, Uanis(C8') \\sim Ueq, Uanis(C9') \\sim Ueq,
Uanis(C10') \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C15') \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(N1') \\sim Ueq, Uanis(C1') \\sim Ueq, Uanis(C2') \\sim Ueq, Uanis(C3')
\\sim Ueq, Uanis(C4') \\sim Ueq, Uanis(C5') \\sim Ueq, Uanis(C6') \\sim Ueq,
Uanis(C7) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.002
Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C16') \\sim Ueq, Uanis(C11')
\\sim Ueq, Uanis(C12') \\sim Ueq, Uanis(C13') \\sim Ueq, Uanis(C14') \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(C16) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(N3)
\\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(S3') \\sim Ueq,
Uanis(S3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(C53) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(N16) \\sim Ueq, Uanis(C65)
\\sim Ueq, Uanis(O9') \\sim Ueq, Uanis(F8') \\sim Ueq, Uanis(F9') \\sim Ueq, :
with sigma of 0.005 and sigma for terminal atoms of 0.002
4. Others
 Sof(N1')=Sof(H1')=Sof(C1')=Sof(C2')=Sof(C3')=Sof(C4')=Sof(H4')=Sof(C5')=
 Sof(H5')=Sof(C6')=Sof(H6')=Sof(C7')=Sof(H7')=Sof(C8')=Sof(C9')=Sof(C10')=
 Sof(C16')=Sof(C11')=Sof(C12')=Sof(H12')=Sof(C13')=Sof(H13')=Sof(C14')=
 Sof(H14')=Sof(C15')=Sof(H15')=1-FVAR(1)
 Sof(N1)=Sof(H1)=Sof(C2)=Sof(C3)=Sof(C8)=Sof(C9)=Sof(C10)=Sof(C1)=Sof(C4)=
 Sof(H4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=Sof(C11)=Sof(C12)=
 Sof(H12)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=FVAR(1)
 Sof(S3')=Sof(F7')=Sof(F8')=Sof(F9')=Sof(O7')=Sof(O8')=Sof(O9')=Sof(C67')=1-
 FVAR(2)
 Sof(S3)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(O7)=Sof(O8)=Sof(O9)=Sof(C67)=FVAR(2)
 Fixed Uiso: F7(0.08) F7'(0.06) F8(0.08) F9(0.08) O7'(0.08) C67(0.08) C67'(0.06)
5.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N1'(H1'), C4(H4), C4'(H4'), C5(H5), C5'(H5'), C6(H6), C6'(H6'),
 C7(H7), C7'(H7'), C12(H12), C13(H13), C14(H14), C15(H15), C12'(H12'),
 C13'(H13'), C14'(H14'), C15'(H15'), C18(H18), C19(H19), C20(H20), C24(H24),
 C25(H25), C26(H26), C30(H30), C31(H31), C32(H32), C36(H36), C37(H37), C38(H38),
  C42(H42), C43(H43), C44(H44), C48(H48), C49(H49), C50(H50), C54(H54),
 C55(H55), C56(H56), C60(H60), C61(H61), C62(H62)
5.b Fitted hexagon refined as free rotating group:
 C2(C3,C8,C9,C10,C1), C11(C12,C13,C14,C15,C16), C16'(C11',C12',C13',C14',C15')
5.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C28(H28A,H28B,H28C), C34(H34A,H34B,H34C), C40(H40A,H40B,
 H40C), C46(H46A,H46B,H46C), C52(H52A,H52B,H52C), C58(H58A,H58B,H58C), C64(H64A,
 H64B,H64C)
;
_shelx_res_checksum              93564
_shelx_fab_checksum              22631
_olex2_submission_special_instructions 'No special instructions were received'