Keggin-type polyoxometalate 1 : 1 complexes of Pb(II) and Bi(III): experimental, theoretical and luminescence studies.
Mukhacheva, Anna A.; Asanova, Tatiana; Ryzhikov, Maxim R.; Sukhikh, Taisiya S.; Kompankov, Nikolay B.; Yanshole, Vadim V.; Berezin, Alexey S.; Gushchin, Artem L.; Abramov, Pavel A.; Sokolov, Maxim N.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 6913–6922; doi:10.1039/d1dt00499a

data_7707095
_publ_section_title
;
 Keggin-type polyoxometalate 1&#x2009;:&#x2009;1 complexes of Pb(II) and
 Bi(III): experimental, theoretical and luminescence studies.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6913
_journal_page_last               6922
_journal_paper_doi               10.1039/d1dt00499a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'(Bi1 K6.17 O90.33 P2 W22 H0.83), 6.33(O H2), 4(C4 H12 N)'
_chemical_formula_sum            'C16 H61.5 Bi K6.17 N4 O96.67 P2 W22'
_chemical_formula_weight         6413.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-01-11 deposited with the CCDC.	2021-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.593(2)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   48.525(3)
_cell_length_b                   12.6920(8)
_cell_length_c                   56.670(3)
_cell_measurement_reflns_used    9725
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.95
_cell_measurement_theta_min      2.36
_cell_volume                     32881(3)
_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(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_unetI/netI     0.0869
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       67
_diffrn_reflns_limit_l_min       -67
_diffrn_reflns_number            90876
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.133
_diffrn_reflns_theta_max         25.133
_diffrn_reflns_theta_min         1.665
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    24.953
_exptl_absorpt_correction_T_max  0.2586
_exptl_absorpt_correction_T_min  0.1485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1409 before and 0.0950 after correction. The Ratio of minimum to maximum transmission is 0.5742. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.879
_exptl_crystal_description       prism
_exptl_crystal_F_000             33642
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.233
_refine_diff_density_min         -2.124
_refine_diff_density_rms         0.452
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1867
_refine_ls_number_reflns         28621
_refine_ls_number_restraints     390
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0722
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+6067.6646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1390
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21745
_reflns_number_total             28621
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00499a2.cif
_cod_data_source_block           akl548
_cod_depositor_comments          'Adding full bibliography for 7707095.cif.'
_cod_database_code               7707095
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.189
_shelx_estimated_absorpt_t_min   0.154
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N5-C20
 1.5 with sigma of 0.02
 C11-C12 \\sim C12-C10 \\sim C12-C9
 with sigma of 0.02
 C24-N6 \\sim C24-N6 \\sim C21-N6 \\sim C23-N6
 with sigma of 0.02
 C24-C21 \\sim C24-C22 \\sim C24-C23 \\sim C22-C21 \\sim C22-C23 \\sim C21-C23
 with sigma of 0.04
 C26-N7 \\sim C26-N7 \\sim C25-N7 \\sim C27-N7
 with sigma of 0.02
 C26-C25 \\sim C26-C28 \\sim C26-C27 \\sim C28-C25 \\sim C28-C27 \\sim C25-C27
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
N6 \\sim C24 \\sim C22 \\sim C21 \\sim C23: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
N7 \\sim C26 \\sim C28 \\sim C25 \\sim C27: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(O92) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O34)
\\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O88) \\sim Ueq, Uanis(O37) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O70) \\sim Ueq, Uanis(O68) \\sim Ueq, Uanis(O76) \\sim Ueq, Uanis(O60)
\\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O106) \\sim Ueq,
Uanis(O118) \\sim Ueq, Uanis(O113) \\sim Ueq, Uanis(O89) \\sim Ueq, Uanis(O91)
\\sim Ueq, Uanis(O101) \\sim Ueq, Uanis(O97) \\sim Ueq, Uanis(O94) \\sim Ueq,
Uanis(O86) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(O64) \\sim Ueq, Uanis(O20)
\\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(O31) \\sim Ueq, Uanis(O49) \\sim Ueq,
Uanis(O69) \\sim Ueq, Uanis(O71) \\sim Ueq, Uanis(O80) \\sim Ueq, Uanis(O85)
\\sim Ueq, Uanis(O117) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(O123) \\sim Ueq,
Uanis(K12) \\sim Ueq, Uanis(K9) \\sim Ueq, Uanis(O75) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O14) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O15)
\\sim Ueq, Uanis(O112) \\sim Ueq, Uanis(O144) \\sim Ueq, Uanis(O114) \\sim Ueq,
Uanis(O74) \\sim Ueq, Uanis(O40) \\sim Ueq, Uanis(O72) \\sim Ueq, Uanis(O153)
\\sim Ueq, Uanis(O93) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O87) \\sim Ueq,
Uanis(O13) \\sim Ueq, Uanis(O59) \\sim Ueq, Uanis(O105) \\sim Ueq, Uanis(O154)
\\sim Ueq, Uanis(O128) \\sim Ueq, Uanis(O45) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uiso(O10) = Uiso(O124)
Uiso(C24) = Uiso(N6) = Uiso(C22) = Uiso(C23) = Uiso(N7) = Uiso(C26) = Uiso(C28)
= Uiso(C21) = Uiso(C25) = Uiso(C27)
4. Rigid body (RIGU) restrains
 N6, C24, C22, C21, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N7, C26, C28, C25, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(N7)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C28)=Sof(H28A)=Sof(H28B)=
 Sof(H28C)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C27)=Sof(H27A)=Sof(H27B)=
 Sof(H27C)=1-FVAR(1)
 Sof(N6)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C22)=Sof(H22A)=Sof(H22B)=
 Sof(H22C)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C23)=Sof(H23A)=Sof(H23B)=
 Sof(H23C)=FVAR(1)
 Fixed Sof: K7(0.5) K9(0.5) K11(0.25) K10(0.5) K12(0.5) O154(0.5) O10(0.33333)
 O134(0.5) O124(0.16667) O16(0.5) O132(0.5) O141(0.5) O142(0.5) O30(0.5)
 O133(0.5) O146(0.5)
6.a Free rotating group:
 N6(C24,C22,C21,C23), N7(C26,C28,C25,C27)
6.b Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,
 H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C),
 C24(H24A,H24B,H24C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C23(H23A,H23B,
 H23C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C25(H25A,H25B,H25C), C27(H27A,
 H27B,H27C)
;
_shelx_res_checksum              23312
_shelx_hkl_checksum              26405
_olex2_submission_special_instructions 'No special instructions were received'