A Dawson-type {P<sub>4</sub>W<sub>24</sub>} modified using phenylphosphonic acid with excellent proton conductivity.
Liu, Jiayu; Lei, Wenjing; Zhang, Shihao; Li, Huafeng; Liu, Siyu; Ma, Pengtao; Wang, Jingping; Niu, Jingyang; Dalton transactions (Cambridge, England : 2003) 53 (2024) 16212–16218; doi:10.1039/d4dt01775g

data_7716993
_publ_section_title
;
 A Dawson-type {P<sub>4</sub>W<sub>24</sub>} modified using
 phenylphosphonic acid with excellent proton conductivity.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16212
_journal_page_last               16218
_journal_paper_doi               10.1039/d4dt01775g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         '0.5(C24 H20 Co4 K10 Na8 O208 P12 W48), 5(O)'
_chemical_formula_sum            'C12 H10 Co2 K5 Na4 O109 P6 W24'
_chemical_formula_weight         6901.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-06-09 deposited with the CCDC.	2024-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.1220(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.2452(9)
_cell_length_b                   21.1687(5)
_cell_length_c                   21.4434(4)
_cell_measurement_reflns_used    9435
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.278
_cell_measurement_theta_min      2.211
_cell_volume                     15998.8(6)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      150.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Helios multilayer optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_unetI/netI     0.0663
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            52886
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         1.899
_diffrn_source_type              Microfocus
_exptl_absorpt_coefficient_mu    17.658
_exptl_absorpt_correction_T_max  0.0167
_exptl_absorpt_correction_T_min  0.0030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1577 before and 0.0736 after correction. The Ratio of minimum to maximum transmission is 0.1796. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.865
_exptl_crystal_description       block
_exptl_crystal_F_000             12052
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         4.790
_refine_diff_density_min         -3.188
_refine_diff_density_rms         0.593
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         14645
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0845
_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^)+(0.1748P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2179
_refine_ls_wR_factor_ref         0.2356
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10903
_reflns_number_total             14645
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01775g2.cif
_cod_data_source_block           m11502_0m_a
_cod_depositor_comments          'Adding full bibliography for 7716993.cif.'
_cod_database_code               7716993
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.332
_shelx_estimated_absorpt_t_min   0.143
_diffrn_source_source            'Incoatc Ius 3.0 '
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 Co2, O5W
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3: within 1.6A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C4 \\sim C5 \\sim C6: within 1.6A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O2W \\sim Co1 \\sim Co1B: within 2.2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O5W \\sim Co2 \\sim Co2B: within 2.2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O10W) \\sim Ueq, Uanis(O9W) \\sim Ueq, Uanis(O11W) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(O5W) \\sim Ueq,
Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: Co1(0.35) Co1B(0.15) Co2(0.35) Co2B(0.15)
5.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4), C3(H3), C2(H2)
5.b Fitted hexagon refined as free rotating group:
 C1(C6,C5,C4,C3,C2)
;
_shelx_res_checksum              13308
_shelx_hkl_checksum              54145
_shelx_fab_checksum              7740
_olex2_submission_special_instructions 'No special instructions were received'