Hard and Soft Metal Complexes of Calix[4]-bis-monothiacrown-5: X-ray and NMR Studies of Discrete Homodinuclear Complexes and a Heteromultinuclear Network
Ja-Yeon Kim; In-Hyeok Park; Jai Young Lee; Joon-Hwa Lee; Ki-Min Park; Shim Sung Lee; Inorganic Chemistry 52 (2013) 10176–10182; doi:10.1021/ic401648b

data_4335909
_publ_section_title
;
 Hard and Soft Metal Complexes of Calix[4]-bis-monothiacrown-5: X-ray and
 NMR Studies of Discrete Homodinuclear Complexes and a Heteromultinuclear
 Network
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10176
_journal_page_last               10182
_journal_paper_doi               10.1021/ic401648b
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C22 H26 Hg2 I5 K O4 S '
_chemical_formula_sum            'C22 H26 Hg2 I5 K O4 S'
_chemical_formula_weight         1461.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.9050(5)
_cell_length_b                   15.0495(2)
_cell_length_c                   13.8112(2)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.68
_cell_measurement_theta_min      2.40
_cell_volume                     6423.66(16)
_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  0.0764
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            69483
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    14.575
_exptl_absorpt_correction_T_max  0.3705
_exptl_absorpt_correction_T_min  0.1366
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.022
_exptl_crystal_description       plate
_exptl_crystal_F_000             5200
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.692
_refine_diff_density_min         -1.894
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         6321
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0258P)^2^+28.8264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0739
_reflns_number_gt                5089
_reflns_number_total             6321
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401648b_si_002_3.cif
_cod_data_source_block           3
_cod_database_code               4335909