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_1548380
_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         'C56 H48 Ag5 N17, 2(C F3 O3 S)'
_chemical_formula_sum            'C58 H48 Ag5 F6 N17 O6 S2'
_chemical_formula_weight         1796.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_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
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.842(6)
_cell_length_b                   21.083(5)
_cell_length_c                   25.145(5)
_cell_measurement_reflns_used    12843
_cell_measurement_temperature    173.15(10)
_cell_measurement_theta_max      31.3642
_cell_measurement_theta_min      1.8677
_cell_volume                     6808(4)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.1303
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            23139
_diffrn_reflns_theta_full        27.63
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         1.86
_diffrn_source                   'fine-focus sealed tube'
_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    1.753
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3536
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.525
_refine_diff_density_min         -5.077
_refine_diff_density_rms         0.288
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         4196
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1871
_refine_ls_R_factor_gt           0.1818
_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^)+(0.0001P)^2^+979.5070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3393
_refine_ls_wR_factor_ref         0.3422
_reflns_number_gt                3913
_reflns_number_total             4196
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7sc04503d2.cif
_cod_data_source_block           y
_cod_depositor_comments
'Adding full bibliography for 1548380--1548386.cif.'
_cod_database_code               1548380
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6-C2
 0.55 with sigma of 0.1
 C2-C4
 2.2 with sigma of 0.1
 N1-C1 \\sim N1-C6
 with sigma of 0.01
3. Rigid bond restraints
 N2, Ag2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
N2 \\sim Ag2: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C4) \\sim Ueq, : with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(Ag2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(N1) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
: with sigma of 0.0005 and sigma for terminal atoms of 0.0005
5. Others
 Fixed Sof: Ag1(0.8) Ag1A(0.1) Ag1B(0.1) Ag2(0.25) N1(0.25) C2(0.25) C3(0.25)
 C6(0.25)
 Fixed Uiso: C2(0.05) C5(0.05)
6.a Me refined with riding coordinates:
 C10(H10A,H10B,H10C), C16(H16A,H16B,H16C)
6.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C12(H12), C13(H13), C14(H14), C18(H18), C19(H19)
;
_olex2_submission_special_instructions 'No special instructions were received'