Employment of a New Tripodal Ligand for the Synthesis of Cobalt(II/III), Nickel(II), and Copper(II) Clusters: Magnetic, Optical, and Thermal Properties
Angelos B. Canaj; Demetrios I. Tzimopoulos; Aggelos Philippidis; George E. Kostakis; Constantinos J. Milios; Inorganic Chemistry 51 (2012) 10461–10470; doi:10.1021/ic301744e

data_4330532
_publ_section_title
;
 Employment of a New Tripodal Ligand for the Synthesis of Cobalt(II/III),
 Nickel(II), and Copper(II) Clusters: Magnetic, Optical, and Thermal
 Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10461
_journal_page_last               10470
_journal_paper_doi               10.1021/ic301744e
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C63.5 H78.5 Cu4 N4 O17.75'
_chemical_formula_weight         1435.96
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2012-08-08 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.89(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.808(9)
_cell_length_b                   26.728(9)
_cell_length_c                   13.601(7)
_cell_measurement_reflns_used    20576
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      23.39
_cell_measurement_theta_min      1.28
_cell_volume                     7184(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector                 'image plate ( 34 cm diameter )'
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_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  0.2007
_diffrn_reflns_av_sigmaI/netI    0.1844
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            61516
_diffrn_reflns_theta_full        25.78
_diffrn_reflns_theta_max         25.78
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    1.234
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_T_min  0.769
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       plate
_exptl_crystal_F_000             2982
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.223
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       0.0085(5)
_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   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     880
_refine_ls_number_reflns         13579
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1968
_refine_ls_R_factor_gt           0.0809
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0830P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1820
_refine_ls_wR_factor_ref         0.2188
_reflns_number_gt                5209
_reflns_number_total             13579
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301744e_si_002_5.cif
_cod_data_source_block           at384
_cod_original_cell_volume        7184(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C63.50 H78.50 Cu4 N4 O17.75'
_cod_database_code               4330532