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_4335908
_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
'C44 H52 Ag2 O8 S2, 2(Cl O4), 2(C H4 O), H2 O'
_chemical_formula_sum            'C46 H62 Ag2 Cl2 O19 S2'
_chemical_formula_weight         1269.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 101.761(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0637(6)
_cell_length_b                   20.6280(10)
_cell_length_c                   22.5805(11)
_cell_measurement_reflns_used    4531
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.26
_cell_measurement_theta_min      2.18
_cell_volume                     5045.2(4)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1376
_diffrn_reflns_av_sigmaI/netI    0.0929
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            77634
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    1.041
_exptl_absorpt_correction_T_max  0.9058
_exptl_absorpt_correction_T_min  0.7876
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_description       block
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.126
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         9920
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1356
_refine_ls_R_factor_gt           0.0730
_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^)+(0.0732P)^2^+20.5848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1616
_refine_ls_wR_factor_ref         0.1940
_reflns_number_gt                5688
_reflns_number_total             9920
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401648b_si_002_2.cif
_cod_data_source_block           2
_cod_database_code               4335908