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_7120260
_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            'C120 Cl8 Cr Mn4 N7 O70 Si2 W18'
_chemical_formula_weight         6580.11
_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                102.4516(6)
_cell_angle_beta                 96.5392(6)
_cell_angle_gamma                93.5466(4)
_cell_formula_units_Z            2
_cell_length_a                   14.32460(10)
_cell_length_b                   20.0905(2)
_cell_length_c                   34.1760(4)
_cell_measurement_reflns_used    42507
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.488
_cell_measurement_theta_min      0.615
_cell_volume                     9503.70(16)
_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 0.961
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_number            50513
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         29.488
_diffrn_reflns_theta_min         0.615
_exptl_absorpt_coefficient_mu    11.349
_exptl_absorpt_correction_T_max  0.750
_exptl_absorpt_correction_T_min  0.356
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL2000 DENZO SCALEPACK'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    2.299
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             5898
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.331
_refine_diff_density_min         -3.883
_refine_diff_density_rms         0.717
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1445
_refine_ls_number_reflns         50513
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1132P)^2^+103.8019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1749
_refine_ls_wR_factor_ref         0.1965
_reflns_Friedel_coverage         0.000
_reflns_number_gt                43988
_reflns_number_total             50513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc04072e2.cif
_cod_data_source_block           p-1
_cod_original_cell_volume        9503.70(17)
_cod_database_code               7120260
_shelxl_version_number           2014/6
_shelx_res_checksum              68333