A water-soluble mixed-valent {Mn<sub>11</sub>} cluster embedded heteropolyoxoniobate with magnetic properties.
Wu, Ping-Xin; Chen, Chun-Xia; Sun, Yan-Qiong; Zheng, Shou-Tian; Chemical communications (Cambridge, England) 60 (2024) 8888–8891; doi:10.1039/d4cc02720e

data_7133388
_publ_section_title
;
 A water-soluble mixed-valent {Mn<sub>11</sub>} cluster embedded
 heteropolyoxoniobate with magnetic properties.
;
_journal_issue                   67
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8888
_journal_page_last               8891
_journal_paper_doi               10.1039/d4cc02720e
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'H237 K25 Mn11 Nb62 O330 Te15'
_chemical_formula_sum            'H237 K25 Mn11 Nb62 O330 Te15'
_chemical_formula_weight         14775.14
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2024-07-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-07-21 deposited with the CCDC.	2024-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                98.666(2)
_cell_angle_beta                 100.990(2)
_cell_angle_gamma                112.911(2)
_cell_formula_units_Z            2
_cell_length_a                   22.620(3)
_cell_length_b                   24.412(3)
_cell_length_c                   38.496(5)
_cell_measurement_reflns_used    9801
_cell_measurement_temperature    175
_cell_measurement_theta_max      25.011
_cell_measurement_theta_min      2.325
_cell_volume                     18617(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       SMART(Bruker,2000)
_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    SHELXTL(Bruker,2000)
_diffrn_ambient_temperature      175
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.0828
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            174520
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.045
_diffrn_reflns_theta_max         25.045
_diffrn_reflns_theta_min         1.558
_exptl_absorpt_coefficient_mu    3.728
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0873 before and 0.0594 after correction.
The Ratio of minimum to maximum transmission is 0.6589.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.636
_exptl_crystal_description       block
_exptl_crystal_F_000             13898
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         4.279
_refine_diff_density_min         -2.015
_refine_diff_density_rms         0.380
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     4194
_refine_ls_number_reflns         65362
_refine_ls_number_restraints     420
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1461
_refine_ls_R_factor_gt           0.0894
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1121P)^2^+1272.4176P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2195
_refine_ls_wR_factor_ref         0.2696
_reflns_Friedel_coverage         0.000
_reflns_number_gt                41366
_reflns_number_total             65362
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02720e2.cif
_cod_data_source_block           a_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7133388.cif.
;
_cod_database_code               7133388
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
O43W \\sim O58W: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(O6) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O10) \\sim
Ueq, Uanis(O20) \\sim Ueq, Uanis(O34) \\sim Ueq, Uanis(O39) \\sim Ueq,
Uanis(O66) \\sim Ueq, Uanis(O79) \\sim Ueq, Uanis(O96) \\sim Ueq, Uanis(O113)
\\sim Ueq, Uanis(O166) \\sim Ueq, Uanis(O212) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(K39) \\sim Ueq, Uanis(O9W) \\sim Ueq, Uanis(K34) \\sim Ueq, Uanis(O14)
\\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(O48) \\sim Ueq, Uanis(O106) \\sim Ueq,
Uanis(O28W) \\sim Ueq, Uanis(O37W) \\sim Ueq, Uanis(O38W) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O23W) \\sim Ueq, Uanis(O27W) \\sim Ueq, Uanis(O29W) \\sim Ueq,
Uanis(O34W) \\sim Ueq, Uanis(O20W) \\sim Ueq, Uanis(O76W) \\sim Ueq,
Uanis(O81W) \\sim Ueq, Uanis(O87W) \\sim Ueq, Uanis(O88W) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O60W) \\sim Ueq, Uanis(O61W) \\sim Ueq, Uanis(O64W) \\sim Ueq,
Uanis(O74W) \\sim Ueq, Uanis(O82W) \\sim Ueq, Uanis(O83W) \\sim Ueq,
Uanis(O85W) \\sim Ueq, Uanis(O90W) \\sim Ueq, Uanis(O36W) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O84W) \\sim Ueq, Uanis(O45W) \\sim Ueq, Uanis(O53W) \\sim Ueq,
Uanis(O68W) \\sim Ueq, Uanis(O78W) \\sim Ueq, Uanis(O97W) \\sim Ueq,
Uanis(O40W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O79W) \\sim Ueq, Uanis(O63W) \\sim Ueq, Uanis(O92W) \\sim Ueq,
Uanis(O91W) \\sim Ueq, Uanis(O96W) \\sim Ueq, Uanis(O50W) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O52W) \\sim Ueq, Uanis(O61W) \\sim Ueq, Uanis(O63W) \\sim Ueq,
Uanis(O94W) \\sim Ueq, Uanis(O95W) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O79W) \\sim Ueq, Uanis(K1) \\sim Ueq, Uanis(K11) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O36W) \\sim Ueq, Uanis(O32W) \\sim Ueq, Uanis(O50W) \\sim Ueq,
Uanis(O46W) \\sim Ueq, Uanis(O28W) \\sim Ueq, Uanis(O57W) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O43W) \\sim Ueq, Uanis(O49W) \\sim Ueq, Uanis(O56W) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(O43W) \\sim Ueq, Uanis(O58W) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O105) \\sim Ueq, Uanis(O21W) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O33W) \\sim Ueq, Uanis(O35W) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Fixed Sof: K11(0.5) K14(0.75) K15(0.5) K16(0.5) K17(0.5) K18(0.5) K19(0.5)
 K20(0.5) K21(0.5) K22(0.5) K39(0.5) K23(0.5) K24(0.5) K25(0.5) K26(0.5)
 K27(0.5) K28(0.5) K29(0.5) K30(0.5) K31(0.5) K32(0.5) K33(0.5) K34(0.5)
 K35(0.5) K36(0.5) K37(0.5) K38(0.5) K1(0.25) H9WA(0.5) H9WB(0.5) O32W(0.75)
 H32A(0.75) H32B(0.75) O36W(0.75) O40W(0.75) O41W(0.5) O43W(0.5) H43A(0.5)
 H43B(0.5) O45W(0.75) O46W(0.5) H46A(0.5) H46B(0.5) O47W(0.75) O50W(0.75)
 H50A(0.75) H50B(0.75) O52W(0.75) H52A(0.75) H52B(0.75) O53W(0.75) H53A(0.75)
 H53B(0.75) O54W(0.75) O55W(0.5) O56W(0.75) H56A(0.75) H56B(0.75) O57W(0.5)
 O58W(0.5) O59W(0.75) H59A(0.75) H59B(0.75) O60W(0.5) O61W(0.5) O62W(0.5)
 O63W(0.5) O64W(0.5) O65W(0.75) O66W(0.75) H66A(0.75) H66B(0.75) O67W(0.5)
 O68W(0.5) O69W(0.5) O70W(0.5) O71W(0.5) O72W(0.5) O73W(0.5) O74W(0.5)
 O75W(0.5) O76W(0.5) O77W(0.5) O78W(0.5) O79W(0.5) H79A(0.5) H79B(0.5)
 O80W(0.5) H80A(0.5) H80B(0.5) O81W(0.5) O82W(0.5) O83W(0.5) O84W(0.5)
 H84A(0.5) H84B(0.5) O85W(0.5) H85A(0.5) H85B(0.5) O86W(0.5) H86A(0.5)
 H86B(0.5) O87W(0.5) H87A(0.5) H87B(0.5) O88W(0.5) O89W(0.5) O90W(0.5)
 H90A(0.5) H90B(0.5) O91W(0.5) O92W(0.5) O93W(0.5) H93A(0.5) H93B(0.5)
 O94W(0.5) O95W(0.25) H95A(0.25) H95B(0.25) O96W(0.5) O97W(0.5)
4.a Free rotating group:
 O9W(H9WA,H9WB), O14W(H14W), O21W(H21A,H21B), O23W(H23A,H23B), O27W(H27W),
 O31W(H31A,H31B), O32W(H32A,H32B), O33W(H33A,H33B), O34W(H34A,H34B), O35W(H35W),
  O38W(H38A,H38B), O39W(H39A,H39B), O46W(H46A,H46B), O50W(H50A,H50B), O53W(H53A,
 H53B), O56W(H56A,H56B), O59W(H59A,H59B), O66W(H66A,H66B), O79W(H79A,H79B),
 O80W(H80A,H80B), O84W(H84A,H84B), O86W(H86A,H86B), O87W(H87A,H87B), O90W(H90A,
 H90B), O93W(H93A,H93B), O95W(H95A,H95B)
4.b Rotating group:
 O26W(H26W), O28W(H28A,H28B), O43W(H43A,H43B), O52W(H52A,H52B), O85W(H85A,H85B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              52712
_shelx_hkl_checksum              77926
_shelx_fab_checksum              532
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20