Encapsulation of the 4-mercaptobenzoate ligand by macrocyclic metal complexes: conversion of a metallocavitand to a metalloligand.
Lach, Jochen; Jeremies, Alexander; Breite, Daniel; Abel, Bernd; Mahns, Benjamin; Knupfer, Martin; Matulis, Vitaly; Ivashkevich, Oleg A.; Kersting, Berthold; Inorganic chemistry 53 (2014) 10825–10834; doi:10.1021/ic500683f

data_4341260
_publ_section_title
;
 Encapsulation of the 4-mercaptobenzoate ligand by macrocyclic metal
 complexes: conversion of a metallocavitand to a metalloligand.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10825
_journal_page_last               10834
_journal_paper_doi               10.1021/ic500683f
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C138 H176 B2 N12 Ni4 O4 S6'
_chemical_formula_weight         2515.73
_space_group_IT_number           2
_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
_cell_angle_alpha                87.781(7)
_cell_angle_beta                 85.210(7)
_cell_angle_gamma                89.109(7)
_cell_formula_units_Z            2
_cell_length_a                   14.2554(11)
_cell_length_b                   23.756(2)
_cell_length_c                   24.402(2)
_cell_measurement_temperature    213(2)
_cell_volume                     8228.1(12)
_computing_cell_refinement       'STOE X-Area'
_computing_data_collection       'STOE X-Area'
_computing_data_reduction        'STOE X-Area'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'STOE IPDS-2T'
_diffrn_measurement_method       hemisphere
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0656
_diffrn_reflns_av_sigmaI/netI    0.1641
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            59968
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  0.8941
_exptl_absorpt_correction_T_min  0.8470
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.015
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2676
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         2.050
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1491
_refine_ls_number_reflns         27303
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1622
_refine_ls_R_factor_gt           0.0869
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1264P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2534
_refine_ls_wR_factor_ref         0.2763
_reflns_number_gt                11090
_reflns_number_total             27303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500683f_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4341260--4341261.cif.'
_cod_original_cell_volume        8228.2(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4341260