Hexavacant γ-Dawson-type phosphotungstates supporting an edge-sharing bis(square-pyramidal) {O<sub>2</sub>M(μ<sub>3</sub>-O)<sub>2</sub>(μ-OAc)MO<sub>2</sub>} core (M = Mn<sup>2+</sup>, Co<sup>2+</sup>, Ni<sup>2+</sup>, Cu<sup>2+</sup>, or Zn<sup>2+</sup>).
Suzuki, Kosuke; Minato, Takuo; Tominaga, Naoto; Okumo, Ichiro; Yonesato, Kentaro; Mizuno, Noritaka; Yamaguchi, Kazuya; Dalton transactions (Cambridge, England : 2003) 48 (2019) 7281–7289; doi:10.1039/c8dt04850a

data_7048969
_publ_section_title
;
 Hexavacant \g-Dawson-type phosphotungstates supporting an edge-sharing
 bis(square-pyramidal)
 {O<sub>2</sub>M(\m<sub>3</sub>-O)<sub>2</sub>(\m-OAc)MO<sub>2</sub>} core
 (M = Mn<sup>2+</sup>, Co<sup>2+</sup>, Ni<sup>2+</sup>, Cu<sup>2+</sup>,
 or Zn<sup>2+</sup>).
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7281
_journal_page_last               7289
_journal_paper_doi               10.1039/c8dt04850a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C54 H9 N5 Ni2 O48 P2 W12'
_chemical_formula_weight         3881.08
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2018-12-06 deposited with the CCDC.
2019-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0988(2)
_cell_length_b                   28.2884(4)
_cell_length_c                   24.8669(3)
_cell_measurement_reflns_used    9850
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.450
_cell_measurement_theta_min      1.286
_cell_volume                     13435.0(3)
_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 0.996
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.075
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_number            9925
_diffrn_reflns_point_group_measured_fraction_full 0.538
_diffrn_reflns_point_group_measured_fraction_max 0.532
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         29.450
_diffrn_reflns_theta_min         1.286
_exptl_absorpt_coefficient_mu    10.584
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.532
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL2000 DENZO SCALEPACK'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.931
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6972
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.897
_refine_diff_density_min         -3.435
_refine_diff_density_rms         0.566
_refine_ls_abs_structure_details
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         9925
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0553
_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^)+(0.1269P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1723
_refine_ls_wR_factor_ref         0.1801
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                8089
_reflns_number_total             9925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04850a2.cif
_cod_data_source_block           Ni2
_cod_depositor_comments
'Adding full bibliography for 7048967--7048971.cif.'
_cod_database_code               7048969
_shelxl_version_number           2014/6
_shelx_res_checksum              44511
_platon_squeeze_void_probe_radius 1.20