New polyoxometalate-based mononuclear lanthanide complexes with slow relaxation of magnetization
Wenzhe Zhou; Xiaojia Feng; Hongshan Ke; Yangguang Li; Jinkui Tang; Enbo Wang; Inorganica Chimica Acta 394 (2013) 770–775; doi:10.1016/j.ica.2012.10.001

data_1512842
_publ_section_title
;
 New polyoxometalate-based mononuclear lanthanide complexes with slow
 relaxation of magnetization
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              770
_journal_page_last               775
_journal_paper_doi               10.1016/j.ica.2012.10.001
_journal_volume                  394
_journal_year                    2013
_chemical_formula_sum            'C48 H52 Ho Mo12 N8 O50 P'
_chemical_formula_weight         2888.16
_space_group_IT_number           126
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2bc'
_symmetry_space_group_name_H-M   'P 4/n n c :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.899(3)
_cell_length_b                   16.899(3)
_cell_length_c                   28.339(6)
_cell_measurement_reflns_used    41734
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      3.05
_cell_volume                     8093(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 0.01
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_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  0.1651
_diffrn_reflns_av_sigmaI/netI    0.0793
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            52857
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.05
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.880
_exptl_absorpt_correction_T_max  0.5966
_exptl_absorpt_correction_T_min  0.5448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR by T.Higashi  8 March, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5528
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.192
_refine_diff_density_min         -1.436
_refine_diff_density_rms         0.182
_refine_ls_extinction_coef       0.00017(7)
_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   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         3564
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0750
_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^)+(0.0903P)^2^+96.8417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1711
_refine_ls_wR_factor_ref         0.1923
_reflns_number_gt                2684
_reflns_number_total             3564
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-394-770-775-4.cif
_cod_data_source_block           t2
_cod_original_sg_symbol_H-M      P4/nnc
_cod_database_code               1512842