Synthesis, Structure, and Ferromagnetic Behavior of Decacopper(II) Cluster Complex Supported by Hexaanionic p-tert-Butylthiacalix[6]arene
Takashi Kajiwara; Noriyoshi Kon; Shuichi Yokozawa; Tasuku Ito; Nobuhiko Iki; Sotaro Miyano; Journal of the American Chemical Society 124 (2002) 11274–11275; doi:10.1021/ja0273391

data_4115170
_publ_section_title
;
 Synthesis, Structure, and Ferromagnetic Behavior of Decacopper(II)
 Cluster Complex Supported by Hexaanionic p-tert-Butylthiacalix[6]arene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11274
_journal_page_last               11275
_journal_paper_doi               10.1021/ja0273391
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C146 H206 Cu10 N8 O33 S12'
_chemical_formula_weight         3621.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 97.659(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.043(3)
_cell_length_b                   17.1273(18)
_cell_length_c                   35.197(4)
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      1.53
_cell_volume                     17949(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
SIR97: a new tool for crystal structure determination and refinement, 
Altomare, A.; Burla, M. C.; Camalli, M.; Cascarano, G.; Giacovazzo, C.; 
Guagliardi, A.; Moliterni, A. G. G.; Polidori, G.; Spagna, R.   
J. Appl. Cryst. 1998, 32, 115. (Sheldrick, 1990)' 
;
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0723
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            57629
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    1.364
_exptl_absorpt_correction_T_max  0.7267
_exptl_absorpt_correction_T_min  0.6467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            'deep red'
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       prism
_exptl_crystal_F_000             7536
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1043
_refine_ls_number_reflns         20437
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.934
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0573
_refine_ls_shift/su_max          2.065
_refine_ls_shift/su_mean         0.091
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1055P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.1803
_reflns_number_gt                12441
_reflns_number_total             20437
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0273391_s2.cif
_cod_data_source_block           decacopper(II)
_cod_original_cell_volume        17950(3)
_cod_database_code               4115170