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_1548386
_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_absolute_configuration ad
_chemical_formula_moiety         'C56 H53 Ag5 N17, 2(C F3 O3 S)'
_chemical_formula_sum            'C58 H53 Ag5 F6 N17 O6 S2'
_chemical_formula_weight         1801.64
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-06-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-06-28 deposited with the CCDC.
2017-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90.00(3)
_cell_angle_beta                 117.31(3)
_cell_angle_gamma                90.00(3)
_cell_formula_units_Z            2
_cell_length_a                   12.278(3)
_cell_length_b                   25.145(5)
_cell_length_c                   12.408(3)
_cell_measurement_reflns_used    12843
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      31.3642
_cell_measurement_theta_min      1.8667
_cell_volume                     3403.7(16)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution
;
????
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 4.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 45.0552
              2theta: -20.3977
scan:
    Number of images: 240
               Slice: -110.0000 - 10.0000
         Image width: 0.5000
            Exp time: 4.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 45.0552
              2theta: -20.3977
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0678
_diffrn_orient_matrix_UB_12      0.0227
_diffrn_orient_matrix_UB_13      -0.0574
_diffrn_orient_matrix_UB_21      -0.0190
_diffrn_orient_matrix_UB_22      0.0337
_diffrn_orient_matrix_UB_23      -0.0091
_diffrn_orient_matrix_UB_31      0.0690
_diffrn_orient_matrix_UB_32      0.0481
_diffrn_orient_matrix_UB_33      0.0340
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1303
_diffrn_reflns_av_unetI/netI     0.0842
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17911
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.81
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    1.551
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6445
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1778
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.377
_refine_diff_density_min         -1.447
_refine_diff_density_rms         0.169
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.21(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1673
_refine_ls_number_reflns         17911
_refine_ls_number_restraints     184
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0889
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1002P)^2^+36.2450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2180
_refine_ls_wR_factor_ref         0.2260
_reflns_number_gt                15934
_reflns_number_total             17911
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7sc04503d2.cif
_cod_data_source_block           y_CCDC5
_cod_depositor_comments
'Adding full bibliography for 1548380--1548386.cif.'
_cod_original_cell_volume        3403.6(12)
_cod_database_code               1548386
_diffrn_number_total             7969
_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. Rigid bond restraints
 C57, C58, C85, C84, C108, C109, C109, C110, S2, C114, S3, C115
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
C57 \\sim C58 \\sim C85 \\sim C84 \\sim C108 \\sim C109 \\sim C109 \\sim C110
\\sim S2 \\sim C114 \\sim S3 \\sim C115: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C51) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(N18)
\\sim Ueq, Uanis(C107) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C113) \\sim Ueq,
Uanis(C2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(C110) \\sim Ueq, Uanis(C84)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C59) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C61)
\\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(N18) \\sim Ueq,
Uanis(C111) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(N23) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.005
Uanis(C3) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
4.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C16(H16), C17(H17), C18(H18), C22(H22), C23(H23), C24(H24), C28(H28), C29(H29),
  C30(H30), C34(H34), C35(H35), C36(H36), C40(H40), C41(H41), C42(H42),
 C46(H46), C47(H47), C48(H48), C52(H52), C53(H53), C54(H54), N18(H18A),
 C60(H60), C61(H61), C62(H62), C63(H63), C66(H66), C67(H67), C68(H68), C72(H72),
  C73(H73), C74(H74), C78(H78), C79(H79), C80(H80), C86(H86), C85(H85),
 C84(H84), C90(H90), C91(H91), C92(H92), C96(H96), C97(H97), C98(H98),
 C102(H102), C103(H103), C104(H104), C108(H108), C109(H109), C110(H110)
4.b Fitted hexagon refined as free rotating group:
 C3(C4,C5,C6,C7,C8), C64(C59,C60,C61,C62,C63), C83(N25,C87,C86,C85,C84)
4.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C20(H20A,H20B,H20C), C26(H26A,H26B,H26C), C32(H32A,H32B,
 H32C), C38(H38A,H38B,H38C), C44(H44A,H44B,H44C), C50(H50A,H50B,H50C), C56(H56A,
 H56B,H56C), C70(H70A,H70B,H70C), C76(H76A,H76B,H76C), C82(H82A,H82B,H82C),
 C88(H88A,H88B,H88C), C94(H94A,H94B,H94C), C100(H10A,H10B,H10C), C106(H10D,H10E,
 H10F), C112(H11A,H11B,H11C)
;
_olex2_submission_special_instructions 'No special instructions were received'