Rhombus-Shaped Tetranuclear [Ln4] Complexes [Ln = Dy(III) and Ho(III)]: Synthesis, Structure, and SMM Behavior
Vadapalli Chandrasekhar; Sakiat Hossain; Sourav Das; Sourav Biswas; Jean-Pascal Sutter; Inorganic Chemistry 52 (2013) 6346–6353; doi:10.1021/ic302848k

data_4335007
_publ_section_title
;
 Rhombus-Shaped Tetranuclear [Ln4] Complexes [Ln = Dy(III) and Ho(III)]:
 Synthesis, Structure, and SMM Behavior
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6346
_journal_page_last               6353
_journal_paper_doi               10.1021/ic302848k
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C34 H22 Ho4 N8 O18, 6(CH3OH), 4(H2O)'
_chemical_formula_sum            'C40 H54 Ho4 N8 O28'
_chemical_formula_weight         1754.03
_chemical_name_systematic
; 
 ? 
;
_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                105.040(6)
_cell_angle_beta                 91.041(7)
_cell_angle_gamma                104.007(7)
_cell_formula_units_Z            1
_cell_length_a                   10.431(4)
_cell_length_b                   11.430(4)
_cell_length_c                   11.838(4)
_cell_measurement_temperature    100(2)
_cell_volume                     1317.6(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0482
_diffrn_reflns_av_sigmaI/netI    0.1084
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7042
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    6.037
_exptl_absorpt_correction_T_max  0.547
_exptl_absorpt_correction_T_min  0.423
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.186
_exptl_crystal_description       block
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.733
_refine_diff_density_min         -3.028
_refine_diff_density_rms         0.463
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         4809
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.1299
_refine_ls_R_factor_gt           0.0855
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1596P)^2^+20.7035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2179
_refine_ls_wR_factor_ref         0.2797
_reflns_number_gt                3116
_reflns_number_total             4809
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302848k_si_001_2.cif
_cod_data_source_block           Complex2
_cod_database_code               4335007