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_1548381
_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_sum            'C59 H55 Ag5 F6 N17 O6 S2'
_chemical_formula_weight         1815.67
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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_method           SHELXL-97
_audit_update_record
;
2017-06-28 deposited with the CCDC.
2017-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                101.197(2)
_cell_angle_beta                 93.200(2)
_cell_angle_gamma                94.368(2)
_cell_formula_units_Z            2
_cell_length_a                   14.3867(3)
_cell_length_b                   15.4794(3)
_cell_length_c                   18.9913(6)
_cell_measurement_reflns_used    14229
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      75.7510
_cell_measurement_theta_min      4.4020
_cell_volume                     4125.97(18)
_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_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.00(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'four-circle diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'micro-focus sealed X-ray tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_sigmaI/netI    0.0878
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15629
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         70.00
_diffrn_reflns_theta_min         3.76
_exptl_absorpt_coefficient_mu    10.375
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19397
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Pale-yellow
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1794
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.727
_refine_diff_density_min         -3.202
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     915
_refine_ls_number_reflns         15629
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0884
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1741P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2452
_refine_ls_wR_factor_ref         0.2632
_reflns_number_gt                12054
_reflns_number_total             15629
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7sc04503d2.cif
_cod_data_source_block           y_CCDC1
_cod_depositor_comments
'Adding full bibliography for 1548380--1548386.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1548381