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_4335907
_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 K2 O8 S2, Cd2 I6, C H2 Cl2'
_chemical_formula_sum            'C45 H54 Cd2 Cl2 I6 K2 O8 S2'
_chemical_formula_weight         1922.30
_chemical_name_systematic
; 
 ? 
;
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_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                   26.2226(18)
_cell_length_b                   14.8423(11)
_cell_length_c                   30.408(2)
_cell_measurement_reflns_used    8327
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      2.18
_cell_volume                     11834.9(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0780
_diffrn_reflns_av_sigmaI/netI    0.0702
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            65330
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    4.196
_exptl_absorpt_correction_T_max  0.8304
_exptl_absorpt_correction_T_min  0.3066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.158
_exptl_crystal_F_000             7248
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.230
_refine_diff_density_min         -1.835
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         14692
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.094
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+34.8268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1262
_reflns_number_gt                9488
_reflns_number_total             14692
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401648b_si_002_1.cif
_cod_data_source_block           1
_cod_original_cell_volume        11835.1(15)
_cod_database_code               4335907