Sequential Synthesis of 3d-3d'-4f Heterometallic Heptanuclear Clusters in between Lacunary Polyoxometalates.
Sato, Rinta; Suzuki, Kosuke; Minato, Takuo; Yamaguchi, Kazuya; Mizuno, Noritaka; Inorganic chemistry 55 (2016) 2023–2029; doi:10.1021/acs.inorgchem.5b02358

data_4346912
_publ_section_title
;
 Sequential Synthesis of 3d-3d'-4f Heterometallic Heptanuclear Clusters in
 between Lacunary Polyoxometalates.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2023
_journal_page_last               2029
_journal_paper_doi               10.1021/acs.inorgchem.5b02358
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C144 Dy2 Fe Mn4 N13 O80 Si2 W18'
_chemical_formula_weight         7157.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   none
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 112.2021(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.2746(7)
_cell_length_b                   23.7787(6)
_cell_length_c                   33.6356(8)
_cell_measurement_reflns_used    27077
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      29.45
_cell_measurement_theta_min      1.12
_cell_volume                     22418.7(10)
_computing_cell_refinement       HKL2000
_computing_data_collection       'Rigaku CrystalClear'
_computing_data_reduction        HKL2000
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_number            29021
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         29.457
_diffrn_reflns_theta_min         1.123
_exptl_absorpt_coefficient_mu    10.211
_exptl_absorpt_correction_T_max  0.489
_exptl_absorpt_correction_T_min  0.200
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL2000 DENZO SCALEPACK'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.121
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             12852
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_platon_squeeze_details
;
;
_refine_diff_density_max         3.067
_refine_diff_density_min         -3.238
_refine_diff_density_rms         0.619
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     792
_refine_ls_number_reflns         29021
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.1356
_refine_ls_R_factor_gt           0.1067
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1049P)^2^+1290.0724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2669
_refine_ls_wR_factor_ref         0.2822
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20992
_reflns_number_total             29021
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02358_si_003.cif
_cod_data_source_block           IIIFeMn4Dy2
_cod_original_cell_volume        22418.6(9)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4346912
_shelx_estimated_absorpt_t_min   0.428
_shelx_estimated_absorpt_t_max   0.535
_shelxl_version_number           2014/6
_shelx_res_checksum              13783
_shelx_hkl_checksum              74351