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_4133775
_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(Fe26.99 K21.78 Mo8 Na8.17 O965.87 P40 W232), K O2.5, Li, 3.5(O), 0.13(K)'
_chemical_formula_sum            'Fe3.38 K3.86 Li Mo Na1.01 O126.73 P5 W29'
_chemical_formula_weight         7980.10
_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             2019-08-06
_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                   52.361(3)
_cell_length_b                   21.6772(12)
_cell_length_c                   26.1817(16)
_cell_measurement_reflns_used    9366
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.71
_cell_measurement_theta_min      2.35
_cell_volume                     29717(3)
_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  'XL (Sheldrick, 2008)'
_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 0.997
_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  0.0425
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       66
_diffrn_reflns_limit_h_min       -59
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            114401
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.747
_diffrn_reflns_theta_min         0.870
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.005
_exptl_absorpt_correction_T_max  0.2607
_exptl_absorpt_correction_T_min  0.1305
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1333 before and 0.0534 after correction. The Ratio of minimum to maximum transmission is 0.5006. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'light black'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    3.567
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             27618
_exptl_crystal_size_max          0.042
_exptl_crystal_size_mid          0.031
_exptl_crystal_size_min          0.017
_refine_diff_density_max         3.177
_refine_diff_density_min         -4.510
_refine_diff_density_rms         0.530
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1071
_refine_ls_number_reflns         16393
_refine_ls_number_restraints     2412
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0831
_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^)+(0.0129P)^2^+9547.5898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1797
_refine_ls_wR_factor_ref         0.1888
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13980
_reflns_number_total             16393
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10277_si_007.cif
_cod_data_source_block           FeMoImma
_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_database_code               4133775
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.644
_shelx_estimated_absorpt_t_min   0.375
_olex2_refinement_description
;
1. Shared sites
{W1, Mo1}
{W3, Mo3}
{W5, Mo5}
{W6, Mo6}
{W7, Mo7}
{W9, Mo9}
{W10, Mo10}
{W11, Mo11}
{W12, Mo12}
{W13, Mo13}
2. Uiso/Uaniso restraints and constraints
Uanis(O20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O77) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O37) \\sim Ueq, Uanis(O2BA) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Li6D) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O1AA) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O40) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(K5AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Fe4) = Uanis(Fe4B)
Uanis(Fe1) = Uanis(Fe2)
Uanis(Fe3) = Uanis(Fe1)
Uanis(O43) = Uanis(O2BA) = Uanis(Fe4B) = Uanis(Fe4)
Uanis(O81) = Uanis(O0CA)
Uanis(W1) = Uanis(Mo1)
Uanis(W3) = Uanis(Mo3)
Uanis(W5) = Uanis(Mo5)
Uanis(W6) = Uanis(Mo6)
Uanis(W7) = Uanis(Mo7)
Uanis(W9) = Uanis(Mo9)
Uanis(W10) = Uanis(Mo10)
Uanis(W11) = Uanis(Mo11)
Uanis(W12) = Uanis(Mo12)
Uanis(W13) = Uanis(Mo13)
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
 Fixed Sof: W1(0.95) W3(0.95) W5(0.95) W6(0.95) W7(0.95) Mo1(0.05) Mo3(0.05)
 Mo5(0.05) Mo6(0.05) Mo7(0.05) W9(0.95) W10(0.95) W11(0.95) W12(0.95) W13(0.95)
 Mo9(0.05) Mo10(0.05) Mo11(0.05) Mo12(0.05) Mo13(0.05) W14(0.5) W14B(0.5)
 W15(0.5) W15B(0.5) W16(0.5) Fe1(0.5) Fe3(0.2) Fe4(0.15) Fe4B(0.25) Fe5(0.25)
 Fe5B(0.25) K0AA(0.16667) K2B(0.2) P4(0.25) P4B(0.25) P5(0.25) P5B(0.25)
 P6(0.25) O0CA(0.25) O2BA(0.25) Li6D(0.5) O7(0.5) O36(0.5) O37(0.5)
 O39(0.33333) O40(0.25) O41(0.5) O42(0.5) O43(0.2) 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) K78(0.125)
 O4AA(0.25) K5AA(0.0625) O0AA(0.25) O6AA(0.5) O2AA(0.08333) O7AA(0.5)
 O9AA(0.16667) O0BA(0.33333) O3AA(0.33333) O4(0.16667)
;
_shelx_res_checksum              19978
_shelx_hkl_checksum              99925
_shelx_fab_checksum              61248
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'