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_4326079
_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
;
C50 H56 N4 O4 S4, 2(C2 F3 O2)
;
_chemical_formula_sum            'C54 H56 F6 N4 O8 S4'
_chemical_formula_weight         1131.27
_chemical_name_systematic
; 
 ? 
;
_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                98.079(3)
_cell_angle_beta                 96.774(2)
_cell_angle_gamma                95.124(3)
_cell_formula_units_Z            1
_cell_length_a                   8.5075(5)
_cell_length_b                   11.7799(7)
_cell_length_c                   13.6194(7)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.49
_cell_volume                     1334.12(13)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31137
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.257
_exptl_absorpt_correction_T_max  0.9634
_exptl_absorpt_correction_T_min  0.8305
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       block
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.976
_refine_diff_density_min         -2.877
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5253
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.1226
_refine_ls_R_factor_gt           0.1068
_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^)+(0.0702P)^2^+6.1994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2439
_refine_ls_wR_factor_ref         0.2548
_reflns_number_gt                4320
_reflns_number_total             5253
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2009607_si_002_2.cif
_cod_data_source_block           L2
_cod_database_code               4326079