Tunable Metal Oxide Frameworks via Coordination Assembly of Preyssler-Type Molecular Clusters.
Chen, Linfeng; San, Khin A.; Turo, Michael J.; Gembicky, Milan; Fereidouni, Shelir; Kalaj, Mark; Schimpf, Alina M.; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b10277

data_4133773
_publ_section_title
;
 Tunable Metal Oxide Frameworks via Coordination Assembly of
 Preyssler-Type Molecular Clusters.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b10277
_journal_year                    2019
_chemical_formula_moiety
'0.13(Fe28 K22 Li8 Na10 O1002.67 P40 W240), 3(O)'
_chemical_formula_sum            'Fe3.5 K2.75 Li Na1.25 O128.33 P5 W30'
_chemical_formula_weight         8062.37
_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             2019-08-07
_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                   52.178(3)
_cell_length_b                   21.6024(12)
_cell_length_c                   26.1423(16)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.60
_cell_measurement_theta_min      2.16
_cell_volume                     29467(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX CCD'
_diffrn_detector_area_resol_mean 8.0
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker X8 APEX'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1002
_diffrn_reflns_av_unetI/netI     0.0939
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       65
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            81170
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.685
_diffrn_reflns_theta_min         1.223
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.877
_exptl_absorpt_correction_T_max  0.2594
_exptl_absorpt_correction_T_min  0.1489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1106 before and 0.0739 after correction. The Ratio of minimum to maximum transmission is 0.5740. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    3.635
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             27853
_exptl_crystal_size_max          0.048
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.031
_refine_diff_density_max         3.866
_refine_diff_density_min         -3.673
_refine_diff_density_rms         0.479
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     977
_refine_ls_number_reflns         16100
_refine_ls_number_restraints     1587
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1181
_refine_ls_R_factor_gt           0.0722
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+5942.9971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1579
_refine_ls_wR_factor_ref         0.1784
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10440
_reflns_number_total             16100
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10277_si_003.cif
_cod_data_source_block           FeImma
_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/rss-feeds/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 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_formula_sum        'Fe3.50 K2.75 Li Na1.25 O128.33 P5 W30'
_cod_database_code               4133773
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.634
_shelx_estimated_absorpt_t_min   0.364
_olex2_refinement_description
;
1. Shared sites
{K2B, Li1}
2. Uiso/Uaniso restraints and constraints
Uanis(Na1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Na3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6DA) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Fe4B) = Uanis(Fe4A)
Uanis(Fe1) = Uanis(Fe5)
Uanis(Fe3) = Uanis(Fe1)
Uanis(K2B) = Uanis(Li1)
Uanis(O43) = Uanis(O2BA) = Uanis(Fe4A) = Uanis(Fe4B)
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(Fe4B)=0.25*(1-FVAR(2))
 Sof(Fe4A)=0.25*FVAR(2)
 Sof(Fe5)=1-FVAR(2)
 Sof(Fe1)=FVAR(2)
 Fixed Sof: W14(0.5) W14B(0.5) W15(0.5) W15B(0.5) W16(0.5) Fe3(0.1) Fe2A(0.2)
 Fe2B(0.2) K0AA(0.375) K2B(0.5) Na3(0.125) P4(0.25) P4B(0.25) P5(0.25)
 P5B(0.25) P6(0.25) Na1(0.25) Na2(0.25) O0CA(0.25) O2BA(0.25) O6DA(0.25)
 O40(0.5) O41(0.33333) O42(0.33333) O43(0.25) O44(0.5) O69(0.5) O70(0.5)
 O71(0.5) O72(0.5) O73(0.5) O74(0.5) O75(0.5) O76(0.5) O77(0.5) O79(0.5)
 O81(0.25) O82(0.5) O83(0.5) O84(0.5) O85(0.5) O86(0.5) O87(0.5) Li1(0.5)
 O7A(0.25) O3AA(0.25)
;
_shelx_res_checksum              92817
_shelx_hkl_checksum              42574
_shelx_fab_checksum              36885
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'