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_4133776
_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
'0.08(Co33.98 K21.28 O1390 P60 Sm12.51 W360), 1.33(Co0.13 O0.17), 0.67(Co0.81 O4.5), Li, 0.67(Co0.18 O), 5.39(O)'
_chemical_formula_sum            'Co3.57 K1.78 Li O125.11 P5 Sm1.04 W30'
_chemical_formula_weight         8115.06
_space_group_crystal_system      orthorhombic
_space_group_IT_number           67
_space_group_name_Hall           '-C 2a 2'
_space_group_name_H-M_alt        'C m m a'
_audit_creation_date             2019-09-23
_audit_creation_method
;
Olex2 1.2
(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            12
_cell_length_a                   21.6853(16)
_cell_length_b                   79.455(6)
_cell_length_c                   26.2348(19)
_cell_measurement_reflns_used    9672
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.77
_cell_measurement_theta_min      2.22
_cell_volume                     45203(6)
_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      100.15
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 8.258
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_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  0.0714
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       100
_diffrn_reflns_limit_k_min       -100
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            170117
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.795
_diffrn_reflns_theta_min         0.930
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.766
_exptl_absorpt_correction_T_max  0.2607
_exptl_absorpt_correction_T_min  0.1020
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1475 before and 0.0784 after correction. The Ratio of minimum to maximum transmission is 0.3913. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'light pink'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    3.577
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             41921
_exptl_crystal_size_max          0.053
_exptl_crystal_size_mid          0.047
_exptl_crystal_size_min          0.021
_refine_diff_density_max         4.317
_refine_diff_density_min         -3.979
_refine_diff_density_rms         0.639
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1215
_refine_ls_number_reflns         24869
_refine_ls_number_restraints     1788
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0897
_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^)+(0.0001P)^2^+21779.9453P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1924
_refine_ls_wR_factor_ref         0.2033
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20505
_reflns_number_total             24869
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10277_si_009.cif
_cod_data_source_block           CoSmCmme
_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        45202(6)
_cod_original_sg_symbol_Hall     '-C 2b 2'
_cod_original_sg_symbol_H-M      'C m m e'
_cod_database_code               4133776
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.635
_shelx_estimated_absorpt_t_min   0.366
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O020) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O13) \\sim Ueq, Uanis(O6BA) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O013) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O7) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O02E) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O01S) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Li8A) = Uanis(K8)
Uanis(O2) = Uanis(O0AA)
Uanis(Co1) = Uanis(Co3) = Uanis(Co2B) = Uanis(Co4) = Uanis(Co5B) = Uanis(Co2A)
= Uanis(Co5A)
Uanis(K011) = Uanis(Co5D) = Uanis(K01E) = Uanis(K8) = Uanis(K0AA) = Uanis(Co5C)
Uanis(Co1) = Uanis(O14) = Uanis(O2AA)
Uanis(O12) = Uanis(Co5B) = Uanis(O1AA)
Uanis(W00A) = Uanis(W1AA)
Uanis(W004) = Uanis(W2)
Uanis(W006) = Uanis(W0)
Uanis(W008) = Uanis(W1)
Uanis(W00F) = Uanis(W0AA)
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(W0AA)=Sof(W0)=Sof(W1)=Sof(W2)=Sof(W1AA)=1-FVAR(1)
 Sof(W004)=Sof(W006)=Sof(W008)=Sof(W00A)=Sof(W00F)=FVAR(1)
 Fixed Sof: Sm1(0.48) Co1(0.5) K011(0.6) Co5D(0.125) K01E(0.15) Co2B(0.35)
 Co4(0.5) O13(0.5) O16(0.5) O3(0.5) O5(0.5) Li8A(0.75) K0AA(0.4) O0AA(0.375)
 O12(0.75) O2AA(0.5) O14(0.5) O4AA(0.125) O5AA(0.25) O6AA(0.5) O3AA(0.25)
 O7AA(0.25) O8AA(0.25) O0BA(0.25) O2BA(0.5) O3BA(0.5) O5BA(0.5) O4(0.16667)
 O6BA(0.5) O7BA(0.08333) O8BA(0.25) O15(0.5) O8(0.33333) O9BA(0.33333)
 O4BA(0.25) O7(0.16667)
;
_shelx_res_checksum              67363
_shelx_hkl_checksum              5884
_shelx_fab_checksum              93585
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'