Heterometallic thiacalix[4]arene-supported Na2NiII12LnIII2 clusters with vertex-fused tricubane cores (Ln = Dy and Tb)
Kecai Xiong; Xinyi Wang; Feilong Jiang; Yanli Gai; Wentao Xu; Kongzhao Su; Xingjun Li; Daqiang Yuan; Maochun Hong; Chem.Commun. 48 (2012) 7456–; doi:10.1039/c2cc32360e

data_7108019
_publ_section_title
;
 Heterometallic thiacalix[4]arene-supported Na2NiII12LnIII2 clusters with
 vertex-fused tricubane cores (Ln = Dy and Tb)
;
_journal_name_full               Chem.Commun.
_journal_page_first              7456
_journal_paper_doi               10.1039/c2cc32360e
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C186 H272.5 Cl2 Dy2 N15.5 Na2 Ni12 O49 S12'
_chemical_formula_weight         5040.73
_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                 99.774(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.546(2)
_cell_length_b                   30.412(3)
_cell_length_c                   36.028(4)
_cell_measurement_reflns_used    65753
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.4430
_cell_measurement_theta_min      2.0090
_cell_volume                     23265(4)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  Saturn724+
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            191383
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    1.784
_exptl_absorpt_correction_T_max  0.7167
_exptl_absorpt_correction_T_min  0.5355
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             9496
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;

SQUEEZE removed one CH3CN and half dma molecules per formula unit.
This valueis calculated based upon volume/count_electrons analysis
and elemental analyses.
See ref: a) Y. F. Bi, X. T. Wang, W. P. Liao, X. F. Wang, X. W. Wang,
H. J. Zhang and S. Gao, J. Am. Chem. Soc. 2009, 131, 11650;
b)Y. F. Bi, S. C. Du and W. P. Liao, Chem. Commun., 2011, 47, 4724.
;
_refine_diff_density_max         1.994
_refine_diff_density_min         -3.903
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2268
_refine_ls_number_reflns         45039
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0814
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1175P)^2^+240.0062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2348
_refine_ls_wR_factor_ref         0.2379
_reflns_number_gt                41840
_reflns_number_total             45039
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc32360e.txt
_cod_data_source_block           complex_1
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7108019