Novel polynuclear architectures incorporating Co2+ and K+ ions bound by dimethylmalonate anions: Synthesis, structure, and magnetic properties
Ekaterina N. Zorina; Natalya V. Zauzolkova; Aleksei A. Sidorov; Grigory G. Aleksandrov; Anatoly S. Lermontov; Mikhail A. Kiskin; Artem S. Bogomyakov; Vladimir S. Mironov; Vladimir M. Novotortsev; Igor L. Eremenko; Inorganica Chimica Acta 396 (2013) 108–118; doi:10.1016/j.ica.2012.10.016

data_1512996
_publ_section_title
;
 Novel polynuclear architectures incorporating Co2+ and K+ ions bound by
 dimethylmalonate anions: Synthesis, structure, and magnetic properties
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              108
_journal_page_last               118
_journal_paper_doi               10.1016/j.ica.2012.10.016
_journal_volume                  396
_journal_year                    2013
_chemical_formula_sum            'C150 H374 Co36 K6 O226'
_chemical_formula_weight         8150.67
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.0248(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   22.0530(10)
_cell_length_b                   28.8254(14)
_cell_length_c                   24.7174(12)
_cell_measurement_reflns_used    9793
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.49
_cell_measurement_theta_min      2.27
_cell_volume                     15712.5(13)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0634
_diffrn_reflns_av_sigmaI/netI    0.0722
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            144142
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.42
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.036
_exptl_absorpt_correction_T_max  0.8223
_exptl_absorpt_correction_T_min  0.5530
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS v2004/1, Sheldrick, G.M., (2004)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             8384
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.961
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1912
_refine_ls_number_reflns         32087
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0700
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+3.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1950
_refine_ls_wR_factor_ref         0.2180
_reflns_number_gt                26388
_reflns_number_total             32087
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-396-108-118-2.cif
_cod_data_source_block           p
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               1512996