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_4330529
_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            'C34 H38 N4 Ni O6'
_chemical_formula_weight         657.39
_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                110.521(13)
_cell_angle_beta                 103.869(15)
_cell_angle_gamma                103.934(14)
_cell_formula_units_Z            2
_cell_length_a                   8.7371(17)
_cell_length_b                   13.993(2)
_cell_length_c                   15.172(3)
_cell_measurement_reflns_used    6313
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      1.53
_cell_volume                     1575.2(6)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector                 'image plate ( 34 cm diameter )'
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.990
_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  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0983
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9682
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.63
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_T_max  0.8893
_exptl_absorpt_correction_T_min  0.8509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       block
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.192
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         5891
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0813
_reflns_number_gt                3624
_reflns_number_total             5891
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301744e_si_002_2.cif
_cod_data_source_block           at328
_cod_original_cell_volume        1575.3(5)
_cod_database_code               4330529