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_4133771
_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(Bi12.56 Co34.63 K41.29 O1470 P60 W360), 0.67(Co0.92 O7.5), 0.67(Li), 3.58(O)'
_chemical_formula_sum            'Bi1.07 Co3.5 K3.44 Li0.67 O131.08 P5 W30'
_chemical_formula_weight         8335.71
_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             2019-09-04
_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                   21.6852(16)
_cell_length_b                   79.711(6)
_cell_length_c                   26.2481(19)
_cell_measurement_reflns_used    5522
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.70
_cell_measurement_theta_min      2.60
_cell_volume                     45371(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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_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  0.0782
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       96
_diffrn_reflns_limit_k_min       -97
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            336427
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.755
_diffrn_reflns_theta_min         1.245
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    24.561
_exptl_absorpt_correction_T_max  0.2594
_exptl_absorpt_correction_T_min  0.1353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1268 before and 0.0572 after correction. The Ratio of minimum to maximum transmission is 0.5216. 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    3.661
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             43127
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.125
_refine_diff_density_max         3.782
_refine_diff_density_min         -3.529
_refine_diff_density_rms         0.439
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1364
_refine_ls_number_reflns         22491
_refine_ls_number_restraints     2156
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0640
_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^)+(0.0241P)^2^+11301.7910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1416
_refine_ls_wR_factor_ref         0.1504
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18610
_reflns_number_total             22491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10277_si_010.cif
_cod_data_source_block           CoBiCmme
_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_sg_symbol_Hall     '-C 2b 2'
_cod_original_sg_symbol_H-M      'C m m e'
_cod_original_formula_sum        'Bi1.07 Co3.50 K3.44 Li0.67 O131.08 P5 W30'
_cod_database_code               4133771
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.149
_shelx_estimated_absorpt_t_min   0.084
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(W1AA) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O013) \\sim Ueq, Uanis(O4AA) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O4CA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(W1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O5) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Bi1A) \\sim Ueq, Uanis(Bi1) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(Bi1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Bi00) \\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(K019) = Uanis(K01E) = Uanis(K8) = Uanis(K0AA) = Uanis(K18)
Uanis(Co1) = Uanis(O14) = Uanis(O2AA)
Uanis(O12) = Uanis(Co5B) = Uanis(O1AA)
Uanis(Bi00) = Uanis(Bi1A)
Uanis(Bi1) = Uanis(Bi0A)
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
 1*[Sof(Co1)]+1*[Sof(Co3)]+1*[Sof(Co2B)]+1*[Sof(Co4)]+1*[Sof(Co5B)]+1*
 [Sof(Co2A)]+1*[Sof(Co5A)]=2.625 with esd of 0
 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: Bi00(0.24) Bi1(0.5) K019(0.25) K01E(0.25) O13(0.5) O3(0.5)
 O5(0.75) Li8A(0.5) K0AA(0.5) O0AA(0.375) K18(0.3) O12(0.75) O2AA(0.5) O14(0.5)
 O5AA(0.25) O6AA(0.5) O3AA(0.25) O7AA(0.25) O9AA(0.125) O0BA(0.25)
 O1BA(0.16667) O2BA(0.5) O3BA(0.5) O4BA(0.5) O5BA(0.25) O6BA(0.5) O4(0.25)
 O7BA(0.5) O8BA(0.33333) O19(0.25) O9BA(0.5) O8(0.0625) O1CA(0.5) O0CA(0.5)
 O2CA(0.5) O3CA(0.5) O4CA(0.5) O18(0.5) O5CA(0.25) O8AA(0.25) Bi0A(0.03)
 Bi1A(0.015)
;
_shelx_res_checksum              26782
_shelx_hkl_checksum              4680
_shelx_fab_checksum              496
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'