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_4133774
_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(K1.2 Na9.47 Ni24.04 O952 P40 W240), 14.18(O), 2(Li0.3 Na0.05 O0.25), 1.27(K)'
_chemical_formula_sum            'K1.42 Li0.6 Na1.28 Ni3.01 O133.68 P5 W30'
_chemical_formula_weight         8074.85
_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                   52.101(9)
_cell_length_b                   21.545(4)
_cell_length_c                   26.104(5)
_cell_measurement_reflns_used    9725
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.03
_cell_measurement_theta_min      2.45
_cell_volume                     29302(9)
_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 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0649
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       64
_diffrn_reflns_limit_h_min       -64
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            118263
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.048
_diffrn_reflns_theta_min         1.408
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker Microstar FR-592'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    24.020
_exptl_absorpt_correction_T_max  0.2598
_exptl_absorpt_correction_T_min  0.1322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1321 before and 0.0668 after correction. The Ratio of minimum to maximum transmission is 0.5089. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    3.661
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             27932
_exptl_crystal_size_max          0.074
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.031
_refine_diff_density_max         4.156
_refine_diff_density_min         -4.872
_refine_diff_density_rms         0.594
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1006
_refine_ls_number_reflns         15037
_refine_ls_number_restraints     1639
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1215
_refine_ls_R_factor_gt           0.0864
_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^)+(0.0395P)^2^+12593.4590P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1811
_refine_ls_wR_factor_ref         0.2118
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11216
_reflns_number_total             15037
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10277_si_004.cif
_cod_data_source_block           NiImma
_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        'K1.42 Li0.60 Na1.28 Ni3.01 O133.68 P5 W30'
_cod_database_code               4133774
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.632
_shelx_estimated_absorpt_t_min   0.363
_olex2_refinement_description
;
1. Shared sites
{K18, Li18}
2. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq, Uanis(O0BA) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O43) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O8CA) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O3AA) \\sim Ueq, Uanis(O4BA) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O20) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Na2) = Uanis(Li18) = Uanis(K18)
Uanis(Ni4A) = Uanis(Ni4B)
Uanis(O85) = Uanis(W16)
Uanis(Ni2A) = Uanis(Ni2B)
Uanis(Ni1) = Uanis(Ni5) = Uanis(Ni4B) = Uanis(Ni4A) = Uanis(Ni2B) = Uanis(Ni2A)
Uanis(K18) = Uanis(K12)
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
 1*[Sof(K18)]=0.7 with esd of 0.01
 Fixed Sof: W14(0.5) W14B(0.5) W15(0.5) W15B(0.5) W16(0.5) Ni1(0.7) P4(0.25)
 P4B(0.25) P5(0.25) P5B(0.25) P6(0.25) O37(0.5) O39(0.5) Ni5(0.1) 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)
 O82(0.5) O83(0.5) O84(0.5) O85(0.5) O86(0.5) O87(0.5) Na2(0.05) Ni4B(0.2)
 Li18(0.3) K12(0.075) Ni2B(0.2) O43(0.33333) O2AA(0.25) O3AA(0.5) O4AA(0.5)
 O5AA(0.5) O4(0.33333) O7AA(0.5) O8AA(0.25) O0BA(0.5) O4BA(0.25) O2BA(0.25)
 O5BA(0.25) O9BA(0.125) O2(0.5) O7BA(0.5) O8BA(0.4) O0CA(0.16667) O1CA(0.33333)
 O2CA(0.0625) O9AA(0.25) O3CA(0.25) O4CA(0.33333) O5CA(0.25) O7CA(0.5)
 O8CA(0.5) O9CA(0.5)
;
_shelx_res_checksum              35733
_shelx_hkl_checksum              39962
_shelx_fab_checksum              28680
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'