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_4346914
_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            'C122 Cl12 Cu4 F24 Fe Gd2 N6 O78 Si2 W18'
_chemical_formula_weight         7668.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   none
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 100.56
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.6894(2)
_cell_length_b                   20.1629(2)
_cell_length_c                   26.5399(3)
_cell_measurement_reflns_used    28939
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      29.51
_cell_measurement_theta_min      2.16
_cell_volume                     10357.77(19)
_computing_cell_refinement       HKL2000
_computing_data_collection       'Rigaku CrystalClear'
_computing_data_reduction        HKL2000
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_number            28677
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         29.518
_diffrn_reflns_theta_min         2.166
_exptl_absorpt_coefficient_mu    11.309
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6896
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         7.129
_refine_diff_density_min         -7.172
_refine_diff_density_rms         0.296
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         28660
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0948P)^2^+192.2826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.1688
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25142
_reflns_number_total             28660
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02358_si_004.cif
_cod_data_source_block           IIIFeCu4Gd2
_cod_original_cell_volume        10357.81(19)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4346914
_shelx_estimated_absorpt_t_min   0.398
_shelx_estimated_absorpt_t_max   0.398
_shelxl_version_number           2013-3
_shelx_res_checksum              35198
_shelx_hkl_checksum              22681