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_1548384
_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
'C58 H54 Ag5 F3 N17 O3 S, 0.5(C Cl3), C H Cl3, 3(C F3 O3 S), 0.75(O), 0.5(C O)'
_chemical_formula_sum            'C63 H55 Ag5 Cl4.5 F12 N17 O13.25 S4'
_chemical_formula_weight         2317.36
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-06-06
_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                103.51(3)
_cell_angle_beta                 90.23(3)
_cell_angle_gamma                118.57(3)
_cell_formula_units_Z            2
_cell_length_a                   13.189(3)
_cell_length_b                   13.561(3)
_cell_length_c                   28.427(6)
_cell_measurement_reflns_used    13646
_cell_measurement_temperature    173.15(10)
_cell_measurement_theta_max      27.4798
_cell_measurement_theta_min      1.7308
_cell_volume                     4302(2)
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.15(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            52869
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.77
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.447
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5185
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2283
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.608
_refine_diff_density_min         -2.364
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1169
_refine_ls_number_reflns         15156
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0795
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+29.6736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1949
_refine_ls_wR_factor_ref         0.2003
_reflns_number_gt                13790
_reflns_number_total             15156
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7sc04503d2.cif
_cod_data_source_block           y_CCDC4
_cod_depositor_comments
'Adding full bibliography for 1548380--1548386.cif.'
_cod_original_cell_volume        4301.6(16)
_cod_original_formula_sum        'C63 H55 Ag5 Cl4.50 F12 N17 O13.25 S4'
_cod_database_code               1548384
_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
 S5-F13 = S5-F14 = S5-F15
 2.7 with sigma of 0.03
 S5-C62
 1.68 with sigma of 0.02
 C62-F13 = C62-F14 = C62-F15
 1.4 with sigma of 0.02
 O17-C67
 1.38 with sigma of 0.05
 F13-F14 \\sim F14-F15 \\sim F13-F15
 with sigma of 0.02
 S2-F6 \\sim S2-F4 \\sim S2-F5
 with sigma of 0.02
 F6-F4 \\sim F6-F5 \\sim F4-F5
 with sigma of 0.02
 O6-O5 \\sim O5-O4 \\sim O6-O4
 with sigma of 0.02
 C59-O6 \\sim C59-O5 \\sim C59-O4
 with sigma of 0.02
 Cl8-C65 \\sim Cl9-C65 \\sim Cl7-C65
 with sigma of 0.02
 Cl3-C63 \\sim Cl1-C63 \\sim Cl2-C63
 with sigma of 0.02
 Cl1-Cl2 \\sim Cl1-Cl3 \\sim Cl2-Cl3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F5) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O15) \\sim Ueq: with sigma of
0.002 and sigma for terminal atoms of 0.002
4. Others
 Sof(Cl7)=Sof(Cl8)=Sof(Cl9)=Sof(C65)=Sof(H65)=1-FVAR(1)
 Sof(Cl4)=Sof(Cl5)=Sof(Cl6)=Sof(C64)=Sof(H64)=FVAR(1)
 Fixed Sof: Cl1(0.25) Cl2(0.25) Cl3(0.25) C63(0.25) Cl10(0.5) Cl11(0.25)
 C66(0.25) S2(0.75) F4(0.75) F5(0.75) F6(0.75) O4(0.75) O5(0.75) O6(0.75)
 C59(0.75) S4(0.5) F10(0.5) F11(0.5) F12(0.5) O10(0.5) O11(0.5) O12(0.5)
 C61(0.5) S5(0.75) F13(0.75) F14(0.75) F15(0.75) O13(0.75) O14(0.75) O15(0.75)
 C62(0.75) O16(0.25) O17(0.5) C67(0.5) O18(0.25) O19(0.25)
 Fixed Uiso: F15(0.15) C62(0.1)
5.a Ternary CH refined with riding coordinates:
 C64(H64), C65(H65)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13),
 C17(H17), C18(H18), C19(H19), C23(H23), C24(H24), C25(H25), C29(H29), C30(H30),
  C31(H31), C35(H35), C36(H36), C37(H37), C41(H41), C42(H42), C43(H43),
 C47(H47), C48(H48), C49(H49), C53(H53), C54(H54), C55(H55)
5.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C27(H27A,H27B,H27C), C33(H33A,H33B,
 H33C), C39(H39A,H39B,H39C), C45(H45A,H45B,H45C), C51(H51A,H51B,H51C), C57(H57A,
 H57B,H57C)
;
_olex2_submission_special_instructions 'No special instructions were received'