Alkali-Metal-Templated Assembly of Two High-Nuclearity Cobalt Clusters Based on Thiacalix[4]arene
Su, Kongzhao; Jiang, Feilong; Qian, Jinjie; Pang, Jiandong; AL-Thabaiti, Shaeel A.; Bawaked, Salem M.; Mokhtar, Mohamed; Chen, Qihui; Hong, Maochun; Crystal Growth & Design 14 (2014) 5865–; doi:10.1021/cg5010903

data_4512000
_publ_section_title
;
 Alkali-Metal-Templated Assembly of Two High-Nuclearity Cobalt Clusters
 Based on Thiacalix[4]arene
;
_journal_issue                   11
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              5865
_journal_paper_doi               10.1021/cg5010903
_journal_volume                  14
_journal_year                    2014
_chemical_formula_sum            'C550 H608 Cl4 Co48 K2 N16 O144 P12 S48'
_chemical_formula_weight         14705.68
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.6500(10)
_cell_angle_beta                 75.7330(10)
_cell_angle_gamma                70.7830(10)
_cell_formula_units_Z            1
_cell_length_a                   22.8996(4)
_cell_length_b                   24.2213(3)
_cell_length_c                   34.9910(5)
_cell_measurement_temperature    100(2)
_cell_volume                     17618.9(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.5594
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0947
_diffrn_reflns_av_sigmaI/netI    0.1510
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            123955
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         67.50
_diffrn_reflns_theta_min         3.03
_diffrn_standards_number         132266
_exptl_absorpt_coefficient_mu    10.968
_exptl_absorpt_correction_T_max  0.1702
_exptl_absorpt_correction_T_min  0.1375
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7522
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;
SQUEEZE removed 13 disordered CH3OH and 4 disordered DMF
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         1.850
_refine_diff_density_min         -1.003
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3594
_refine_ls_number_reflns         62870
_refine_ls_number_restraints     313
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1397
_refine_ls_R_factor_gt           0.0866
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1353P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2180
_refine_ls_wR_factor_ref         0.2456
_reflns_number_gt                35458
_reflns_number_total             62870
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5010903_si_003.cif
_cod_data_source_block           c:compound2
_cod_depositor_comments
'Adding full bibliography for 4511999--4512000.cif.'
_cod_database_code               4512000