Incorporation of Cr<sup>III</sup> into a Keggin Polyoxometalate as a Chemical Strategy to Stabilize a Labile {Cr<sup>III</sup>O<sub>4</sub>} Tetrahedral Conformation and Promote Unattended Single-Ion Magnet Properties.
Gumerova, Nadiia I.; Roller, Alexander; Giester, Gerald; Krzystek, J.; Cano, Joan; Rompel, Annette; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b12797

data_4134136
_publ_section_title
;
 Incorporation of Cr<sup>III</sup> into a Keggin Polyoxometalate as a
 Chemical Strategy to Stabilize a Labile {Cr<sup>III</sup>O<sub>4</sub>}
 Tetrahedral Conformation and Promote Unattended Single-Ion Magnet
 Properties.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b12797
_journal_year                    2020
_chemical_formula_moiety         'Cr0.6 O40 W12'
_chemical_formula_sum            'Cr0.6 O40 W12'
_chemical_formula_weight         2877.40
_chemical_name_common            'alpha dodecatungstochromate(III)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.788(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.0892(6)
_cell_length_b                   21.1101(6)
_cell_length_c                   13.0805(4)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    104(2)
_cell_measurement_theta_max      72.588
_cell_measurement_theta_min      6.850
_cell_volume                     4117.7(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      103.8
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1363
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            29032
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        65.084
_diffrn_reflns_theta_max         65.083
_diffrn_reflns_theta_min         6.384
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    31.112
_exptl_absorpt_correction_T_max  0.4245
_exptl_absorpt_correction_T_min  0.0554
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;   
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1019 before and 0.0733 after correction.
The Ratio of minimum to maximum transmission is 0.3230.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.321
_exptl_crystal_description       block
_exptl_crystal_F_000             2445
_exptl_crystal_recrystallization_method
'crystallization from aqueous solution'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.113
_refine_diff_density_min         -2.944
_refine_diff_density_rms         0.255
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         3593
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0666
_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^)+(0.0750P)^2^+145.1705P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1802
_refine_ls_wR_factor_ref         0.1857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3148
_reflns_number_total             3593
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12797_si_003.cif
_cod_data_source_block           nagucr127_c2m
_cod_original_formula_sum        'Cr0.60 O40 W12'
_cod_database_code               4134136
_shelx_estimated_absorpt_t_max   0.166
_shelx_estimated_absorpt_t_min   0.166