A modular synthesis approach to multinuclear heterometallic oxo clusters in polyoxometalates
Minato, Takuo; Suzuki, Kosuke; Ohata, Yusuke; Yamaguchi, Kazuya; Mizuno, Noritaka; Chem. Commun.  (2017) –; doi:10.1039/C7CC04072E

data_7120258
_publ_section_title
;
 A modular synthesis approach to multinuclear heterometallic oxo clusters
 in polyoxometalates
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC04072E
_journal_year                    2017
_chemical_formula_sum            'C84 Ag2 Cr Mn4 N7 O70 Si2 W18'
_chemical_formula_weight         6079.89
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   none
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2017-03-29 deposited with the CCDC.
2017-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                68.6210(10)
_cell_angle_beta                 80.4000(10)
_cell_angle_gamma                66.5450(10)
_cell_formula_units_Z            1
_cell_length_a                   14.5907(2)
_cell_length_b                   14.8029(2)
_cell_length_c                   19.3294(3)
_cell_measurement_reflns_used    17229
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.524
_cell_measurement_theta_min      1.132
_cell_volume                     3565.21(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      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.061
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_number            19562
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         29.524
_diffrn_reflns_theta_min         1.132
_exptl_absorpt_coefficient_mu    15.230
_exptl_absorpt_correction_T_max  0.859
_exptl_absorpt_correction_T_min  0.574
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL2000 DENZO SCALEPACK'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.832
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2691
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         9.497
_refine_diff_density_min         -4.002
_refine_diff_density_rms         0.917
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         19562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1212P)^2^+96.9563P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1766
_refine_ls_wR_factor_ref         0.1977
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18222
_reflns_number_total             19562
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc04072e2.cif
_cod_data_source_block           P-1
_cod_original_cell_volume        3565.21(9)
_cod_database_code               7120258
_shelxl_version_number           2014/6
_shelx_res_checksum              69773