Extra Large Macrocycle: 40-Membered Macrocycle via 2:2 Cyclization and Its Dimercury(II) Complex
Daram Jung; Rie Chamura; Yoichi Habata; Shim Sung Lee; Inorganic Chemistry 50 (2011) 8392–8396; doi:10.1021/ic2009607

data_4326078
_publ_section_title
;
 Extra Large Macrocycle: 40-Membered Macrocycle via 2:2 Cyclization and
 Its Dimercury(II) Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8392
_journal_page_last               8396
_journal_paper_doi               10.1021/ic2009607
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety
;
C60 H72 N4 O8 S4
;
_chemical_formula_sum            'C60 H72 N4 O8 S4'
_chemical_formula_weight         1105.46
_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                65.292(2)
_cell_angle_beta                 89.438(2)
_cell_angle_gamma                73.899(2)
_cell_formula_units_Z            1
_cell_length_a                   11.1337(4)
_cell_length_b                   11.4072(4)
_cell_length_c                   12.8970(4)
_cell_measurement_reflns_used    8880
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.73
_cell_measurement_theta_min      2.36
_cell_volume                     1419.04(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22461
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.226
_exptl_absorpt_correction_T_max  0.9866
_exptl_absorpt_correction_T_min  0.8709
_exptl_absorpt_correction_type   multi-scane
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       plate
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0563P)^2^+0.7579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1222
_reflns_number_gt                4569
_reflns_number_total             5570
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2009607_si_002_1.cif
_cod_data_source_block           5b
_cod_original_cell_volume        1419.04(8)
_cod_original_sg_symbol_Hall     '-p 1'
_cod_database_code               4326078