Tetranuclear Ni(II) and Co(II) Schiff-base complexes with an M4O6 defective dicubane-like core: zero-field SMM behavior in the cobalt analogue
Nemec, Ivan; Herchel, Radovan; Machata, Marek; Travnicek, Zdenek; New J. Chem. 41 (2017) 11258–11267; doi:10.1039/C7NJ02281F

data_7056556
_publ_section_title
;
 Tetranuclear Ni(II) and Co(II) Schiff-base complexes with an M4O6
 defective dicubane-like core: zero-field SMM behavior in the cobalt
 analogue
;
_journal_issue                   19
_journal_name_full               'New J. Chem.'
_journal_page_first              11258
_journal_page_last               11267
_journal_paper_doi               10.1039/C7NJ02281F
_journal_volume                  41
_journal_year                    2017
_chemical_formula_sum            'C27 H22 N2 Ni2 O5'
_chemical_formula_weight         571.87
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-12-21 deposited with the CCDC.
2017-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                112.276(5)
_cell_angle_beta                 97.062(4)
_cell_angle_gamma                108.048(4)
_cell_formula_units_Z            2
_cell_length_a                   8.4860(4)
_cell_length_b                   12.0008(7)
_cell_length_c                   12.9636(7)
_cell_measurement_reflns_used    11222
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.128
_cell_measurement_theta_min      2.888
_cell_volume                     1117.37(12)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  ' enCIFer (Allen et al., 2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10609
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.994
_diffrn_reflns_theta_max         24.994
_diffrn_reflns_theta_min         3.056
_exptl_absorpt_coefficient_mu    1.730
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_description       prism
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         3932
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0423P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0767
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3006
_reflns_number_total             3932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj02281f2.cif
_cod_data_source_block           3
_cod_original_cell_volume        1117.36(11)
_cod_database_code               7056556
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.713
_shelx_estimated_absorpt_t_max   0.724
_exptl_absorpt_special_details
;
face-indexed (CrysAlis RED; Oxford Diffraction, 2006)
;
_shelx_res_checksum              4551