Constructing calixarene-supported high nuclearity Co27, Co28and Ni18Na6clusters with triazoles as co-bridges
Wang, Shentang; Bi, Yanfeng; Liao, Wuping; CrystEngComm 17 (2015) 2896–; doi:10.1039/C5CE00314H

data_7219707
_publ_section_title
;
 Constructing calixarene-supported high nuclearity Co27, Co28and
 Ni18Na6clusters with triazoles as co-bridges
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2896
_journal_paper_doi               10.1039/C5CE00314H
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C258 H294 Cl18 N18 Na6 Ni18 O32 S30'
_chemical_formula_sum            'C258 H294 Cl18 N18 Na6 Ni18 O32 S30'
_chemical_formula_weight         6953.73
_chemical_name_common            '[Ni18Na6Cl6(C40H44S4O4)6(C2N3HS)6(H2O)6]'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-02-23 deposited with the CCDC.
2015-02-27 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   23.340(3)
_cell_length_b                   23.340(3)
_cell_length_c                   55.409(11)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.16
_cell_measurement_theta_min      1.070
_cell_volume                     26140(7)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0911
_diffrn_reflns_av_sigmaI/netI    0.0597
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            23616
_diffrn_reflns_theta_full        17.16
_diffrn_reflns_theta_max         17.16
_diffrn_reflns_theta_min         1.10
_exptl_absorpt_coefficient_mu    1.327
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1996'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             10740
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
P. van der Sluis and A. L. Spek, Acta Crystallogr., 1990, A46, 194.

Two CH3OH molecules and four CHCl3 molecules per formula unit 
were removed by the SQUEEZE process, 
which was deduced based on the void_volume/count_electrons results 
and TG analysis.
;
_refine_diff_density_max         1.040
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.155
_refine_ls_extinction_coef       0.00020(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         3479
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.1279
_refine_ls_R_factor_gt           0.1047
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2798
_refine_ls_wR_factor_ref         0.3015
_reflns_number_gt                2494
_reflns_number_total             3479
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00314h2.cif
_cod_data_source_block           CIAC-213
_cod_depositor_comments
'Adding full bibliography for 7219704--7219707.cif.'
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7219707