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_4330528
_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_moiety         'C73 H68 Co5 N4 O16,  8.5(C H4 O)'
_chemical_formula_sum            'C81.5 H102 Co5 N4 O24.5'
_chemical_formula_weight         1824.32
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.442(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.093(2)
_cell_length_b                   18.4290(14)
_cell_length_c                   29.824(4)
_cell_measurement_reflns_used    14439
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      22.59
_cell_measurement_theta_min      1.30
_cell_volume                     8842.3(18)
_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  0.1169
_diffrn_reflns_av_sigmaI/netI    0.1866
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            41941
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    0.992
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       plate
_exptl_crystal_F_000             3800
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1063
_refine_ls_number_reflns         15644
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.2023
_refine_ls_R_factor_gt           0.0850
_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^)+(0.0500P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1528
_refine_ls_wR_factor_ref         0.1884
_reflns_number_gt                6434
_reflns_number_total             15644
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301744e_si_002_1.cif
_cod_data_source_block           at320
_cod_original_cell_volume        8842.1(17)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C81.50 H102 Co5 N4 O24.50'
_cod_database_code               4330528