Controlled assemblies of hepta- and trideca-CoII clusters by a rational derivation of salicylalde schiff bases: microwave-assisted synthesis, crystal structures, ESI-MS solution analysis and magnetic properties
Wei, Lian-Qiang; Li, Bing-Wen; Hu, Sheng; Zeng, Ming-Hua; CrystEngComm 13 (2011) 510–; doi:10.1039/c0ce00085j

data_7205126
_publ_section_title
;
 Controlled assemblies of hepta- and trideca-CoII clusters by a
 rational derivation of salicylalde schiff bases: microwave-assisted
 synthesis, crystal structures, ESI-MS solution analysis and magnetic
 properties
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              510
_journal_paper_doi               10.1039/c0ce00085j
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C126 H131 Cl4 Co13 N14 O58.5'
_chemical_formula_weight         3685.34
_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                97.718(4)
_cell_angle_beta                 100.731(4)
_cell_angle_gamma                99.178(4)
_cell_formula_units_Z            2
_cell_length_a                   12.915(3)
_cell_length_b                   17.707(4)
_cell_length_c                   33.205(7)
_cell_measurement_temperature    293(2)
_cell_volume                     7259(3)
_computing_cell_refinement       'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.'
_computing_data_collection       'SMART Bruker AXS Inc., 1998.'
_computing_data_reduction        'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.'
_computing_molecular_graphics    'SHELXTL Ver. 6.12, (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL Ver. 6.12, (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXTL Ver. 6.12, (Sheldrick, 2000)'
_computing_structure_solution    'SHELXTL Ver. 6.12, (Sheldrick, 2000)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Apex CCd'
_diffrn_measurement_method       '\w scan'
_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  0.0852
_diffrn_reflns_av_sigmaI/netI    0.1986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            38612
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         0.63
_exptl_absorpt_coefficient_mu    1.613
_exptl_absorpt_correction_T_max  0.6699
_exptl_absorpt_correction_T_min  0.5576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.215
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1953
_refine_ls_number_reflns         22600
_refine_ls_number_restraints     98
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.2192
_refine_ls_R_factor_gt           0.0973
_refine_ls_shift/su_max          6.451
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1951
_refine_ls_wR_factor_ref         0.2569
_reflns_number_gt                9225
_reflns_number_total             22600
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CE00085J.TXT
_cod_data_source_block           l1
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C126 H131 Cl4 Co13 N14 O58.50'
_cod_database_code               7205126