Co<sup>2+</sup>-Linked [NaP<sub>5</sub>W<sub>30</sub>O<sub>110</sub>]<sup>14-</sup>: A Redox-Active Metal Oxide Framework with High Electron Density.
Turo, Michael J.; Chen, Linfeng; Moore, Curtis E.; Schimpf, Alina M.; Journal of the American Chemical Society 141 (2019) 4553–4557; doi:10.1021/jacs.9b00866

data_4128922
_publ_section_title
;
 Co<sup>2+</sup>-Linked
 [NaP<sub>5</sub>W<sub>30</sub>O<sub>110</sub>]<sup>14-</sup>: A
 Redox-Active Metal Oxide Framework with High Electron Density.
;
_journal_issue                   11
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4553
_journal_page_last               4557
_journal_paper_doi               10.1021/jacs.9b00866
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety
'0.13(Co32 K28 Li12 Na8 O1000 P40 W240), 1.5(O)'
_chemical_formula_sum            'Co4 K3.5 Li1.5 Na O126.5 P5 W30'
_chemical_formula_weight         8100.32
_space_group_crystal_system      orthorhombic
_space_group_IT_number           74
_space_group_name_Hall           '-I 2b 2'
_space_group_name_H-M_alt        'I m m a'
_audit_creation_date             2018-10-03
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   52.0499(12)
_cell_length_b                   21.5528(5)
_cell_length_c                   26.1891(6)
_cell_measurement_reflns_used    9821
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.282
_cell_measurement_theta_min      2.344
_cell_volume                     29379.5(12)
_computing_cell_refinement       'SAINT v8.38A (Bruker, 2017)'
_computing_data_collection       'APEX3 v2017.3-0 (Bruker, 2017)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 8.258
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Ultra'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       62
_diffrn_reflns_limit_h_min       -62
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            96625
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.405
_diffrn_reflns_theta_min         1.452
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    24.071
_exptl_absorpt_correction_T_max  0.0265
_exptl_absorpt_correction_T_min  0.0074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1404 before and 0.0558 after correction. The Ratio of minimum to maximum transmission is 0.3736. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    3.663
_exptl_crystal_description       block
_exptl_crystal_F_000             27976
_exptl_crystal_size_max          0.076
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.053
_refine_diff_density_max         3.682
_refine_diff_density_min         -4.724
_refine_diff_density_rms         0.419
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1012
_refine_ls_number_reflns         13930
_refine_ls_number_restraints     1917
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0721
_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^)+(0.0644P)^2^+5785.2905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1794
_refine_ls_wR_factor_ref         0.2021
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10524
_reflns_number_total             13930
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b00866_si_003.cif
_cod_data_source_block           reducedImma
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_formula_sum        'Co4 K3.50 Li1.50 Na O126.50 P5 W30'
_cod_database_code               4128922
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.362
_shelx_estimated_absorpt_t_min   0.262
_olex2_refinement_description
;
1. Shared sites
{K2B, Li1}
2. Uiso/Uaniso restraints and constraints
Uanis(Co4A) = Uanis(Co4B)
Uanis(Co1) = Uanis(Co5)
Uanis(Co3) = Uanis(Co1)
Uanis(K2B) = Uanis(Li1)
Uanis(O43) = Uanis(O2BA) = Uanis(Co4B) = Uanis(Co4A)
Uanis(O81) = Uanis(O0CA)
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(Co4A)=0.25*(1-FVAR(2))
 Sof(Co4B)=0.25*FVAR(2)
 Sof(Co5)=1-FVAR(2)
 Sof(Co1)=FVAR(2)
 Fixed Sof: W15B(0.5) W16(0.5) W14(0.5) W14B(0.5) W15(0.5) P5B(0.25) P4B(0.25)
 Na2(0.25) P4(0.25) P5(0.25) P6(0.25) O73(0.5) O76(0.5) O82(0.5) O44(0.5)
 O84(0.5) O69(0.5) O83(0.5) O72(0.5) O75(0.5) O70(0.5) O40(0.5) O42(0.5)
 O41(0.5) Co3(0.25) O79(0.5) O87(0.5) O71(0.5) O85(0.5) O74(0.5) O86(0.5)
 Co2B(0.25) Co2A(0.25) O43(0.25) O77(0.5) Na1(0.25) O2BA(0.25) O0CA(0.25)
 O81(0.25) O6DA(0.25) K3(0.25) K1(0.25) Li1(0.75) K2B(0.25) O78(0.25)
;
_shelx_res_checksum              8306
_shelx_hkl_checksum              78166
_shelx_fab_checksum              73299
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'