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_7219704
_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         'C283 H348 Cl10 Co28 N48 O49 S41'
_chemical_formula_sum            'C283 H348 Cl10 Co28 N48 O49 S41'
_chemical_formula_weight         8525.09
_chemical_name_common
'[Co28(C40H44S4O4)6(C2N3H2S)8(C4N6H2S2)4(SO4)Cl10(OH)4(CH3OH)4(H2O)6]'
_chemical_name_systematic        ?
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_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                 111.6710(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   20.9882(3)
_cell_length_b                   43.6525(6)
_cell_length_c                   24.5435(3)
_cell_measurement_reflns_used    9259
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.7784
_cell_measurement_theta_min      2.2048
_cell_volume                     20897.1(5)
_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      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0980
_diffrn_reflns_av_sigmaI/netI    0.0769
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            175004
_diffrn_reflns_theta_full        21.65
_diffrn_reflns_theta_max         21.65
_diffrn_reflns_theta_min         0.89
_exptl_absorpt_coefficient_mu    1.406
_exptl_absorpt_correction_T_max  0.8275
_exptl_absorpt_correction_T_min  0.7961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ' SADABS, Sheldrick, 1996'
_exptl_crystal_colour            celadon
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8712
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;
P. van der Sluis and A. L. Spek, Acta Crystallogr., 1990, A46, 194.

Seven CH3OH 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         1.668
_refine_diff_density_min         -1.769
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       0.00022(4)
_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   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1772
_refine_ls_number_reflns         24900
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1156
_refine_ls_R_factor_gt           0.0823
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1634P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2396
_refine_ls_wR_factor_ref         0.2600
_reflns_number_gt                15910
_reflns_number_total             24900
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00314h2.cif
_cod_data_source_block           CIAC-210
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3086 2015-02-26 13:12:21Z robertas 

 Adding full bibliography for 7219704--7219707.cif.
;
_cod_original_sg_symbol_H-M      P2(1)/m
_cod_database_code               7219704