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_4133778
_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(K13.83 Li2 Mn26.4 Na19.58 O968 P40 W240), 4(O)'
_chemical_formula_sum            'K1.73 Li0.25 Mn3.3 Na2.44 O125 P5 W30'
_chemical_formula_weight         7977.09
_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                   52.303(8)
_cell_length_b                   21.664(2)
_cell_length_c                   26.055(3)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.92
_cell_measurement_theta_min      2.44
_cell_volume                     29523(6)
_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 0.999
_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  0.0959
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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       25
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            100879
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.034
_diffrn_reflns_theta_max         25.034
_diffrn_reflns_theta_min         1.222
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.743
_exptl_absorpt_correction_T_max  0.2590
_exptl_absorpt_correction_T_min  0.1762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1444 before and 0.0611 after correction. The Ratio of minimum to maximum transmission is 0.6803. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.589
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             27504
_exptl_crystal_size_max          0.055
_exptl_crystal_size_mid          0.041
_exptl_crystal_size_min          0.024
_refine_diff_density_max         3.653
_refine_diff_density_min         -3.406
_refine_diff_density_rms         0.451
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     959
_refine_ls_number_reflns         13581
_refine_ls_number_restraints     1560
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0679
_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^)+(0.0366P)^2^+8229.6895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1607
_refine_ls_wR_factor_ref         0.1751
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9697
_reflns_number_total             13581
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10277_si_002.cif
_cod_data_source_block           MnImma
_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_cell_volume        29522(6)
_cod_original_formula_sum        'K1.73 Li0.25 Mn3.30 Na2.44 O125 P5 W30'
_cod_database_code               4133778
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.635
_shelx_estimated_absorpt_t_min   0.366
_olex2_refinement_description
;
1. Shared sites
{Li0C, Na12}
2. Uiso/Uaniso restraints and constraints
Uanis(O72) \\sim Ueq, Uanis(Mn4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O1CA) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Na12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O0CA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Mn5A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Mn1) = Uanis(Na2)
Uanis(Mn3) = Uanis(Mn1)
Uanis(Li0C) = Uanis(Na12)
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 0.004
4. Others
 Fixed Sof: W14(0.5) W14B(0.5) W15(0.5) W15B(0.5) W16(0.5) Mn1(0.75) Mn3(0.25)
 Mn2(0.15) Mn5B(0.15) P4(0.25) P4B(0.25) P5(0.25) P5B(0.25) P6(0.25)
 Li0C(0.125) Na12(0.125) O85(0.5) O42(0.5) O69(0.5) O72(0.5) O82(0.5) O83(0.5)
 O3AA(0.5) O4AA(0.5) O2AA(0.5) O16(0.5) O9AA(0.5) O8AA(0.5) O6AA(0.5) O7AA(0.5)
 O0BA(0.5) O3BA(0.5) O6BA(0.75) O7BA(0.25) O2(0.25) Mn5A(0.1) O10(0.25)
 O7(0.25) Mn4(0.25)
;
_shelx_res_checksum              1089
_shelx_hkl_checksum              28302
_shelx_fab_checksum              10388
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'