Making a [Co24] metallamacrocycle from the shuttlecock-like tetranuclear cobalt-calixarene building blocks.
Bi, Yanfeng; Xu, Guancheng; Liao, Wuping; Du, Shangchao; Wang, Xinwu; Deng, Ruiping; Zhang, Hongjie; Gao, Song; Chemical communications (Cambridge, England) 46 (2010) 6362–6364; doi:10.1039/c0cc01844a

data_7112984
_publ_section_title
;
 Making a [Co24] metallamacrocycle from the shuttlecock-like tetranuclear
 cobalt-calixarene building blocks.
;
_journal_issue                   34
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6362
_journal_page_last               6364
_journal_paper_doi               10.1039/c0cc01844a
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety
'[Co24Cl12(C40H44S4O4)6(C2N3H2)12(CH3OH)6(H2O)6](CHCl3)13(CH3OH)2'
_chemical_formula_sum            'C285 H345 Cl51 Co24 N36 O38 S24'
_chemical_formula_weight         8874.68
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   28.1842(3)
_cell_length_b                   28.1842(3)
_cell_length_c                   46.3608(6)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.9818
_cell_measurement_theta_min      2.3497
_cell_volume                     31892.8(6)
_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_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            92239
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.94
_exptl_absorpt_coefficient_mu    1.402
_exptl_absorpt_correction_T_max  0.6949
_exptl_absorpt_correction_T_min  0.6705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ' SADABS, Sheldrick, 1996'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             13530
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_platon_squeeze_details
;
P. van der Sluis and A. L. Spek, Acta Crystallogr., 1990, A46, 194.
;
_refine_diff_density_max         1.665
_refine_diff_density_min         -1.720
_refine_diff_density_rms         0.235
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         12498
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1226P)^2^+536.2681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2024
_refine_ls_wR_factor_ref         0.2142
_reflns_number_gt                10103
_reflns_number_total             12498
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc01844a.txt
_cod_data_source_block           Co24
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/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 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_Hall     '-R 3 '
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7112984