Assembly of tetra-nuclear Yb<sup>III</sup>-containing selenotungstate clusters: synthesis, structures, and magnetic properties.
Han, Li-Zhi; Jiao, Cheng-Qi; Chen, Wei-Chao; Shao, Kui-Zhan; Jin, Long-Yi; Su, Zhong-Min; Dalton transactions (Cambridge, England : 2003) 50 (2021) 11535–11541; doi:10.1039/d1dt01282g

data_7707959
_publ_section_title
;
 Assembly of tetra-nuclear Yb<sup>III</sup>-containing selenotungstate
 clusters: synthesis, structures, and magnetic properties.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11535
_journal_page_last               11541
_journal_paper_doi               10.1039/d1dt01282g
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'H28 Na O176 Se6 W45 Yb4,4(C2 H8 N)??38??H2O????13??Na??'
_chemical_formula_sum            'C8 H136 N4 Na14 O214 Se6 W45 Yb4'
_chemical_formula_weight         13474.23
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-15 deposited with the CCDC.	2021-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                93.153(2)
_cell_angle_beta                 99.868(2)
_cell_angle_gamma                106.3400(10)
_cell_formula_units_Z            2
_cell_length_a                   17.1503(13)
_cell_length_b                   25.5807(19)
_cell_length_c                   35.868(3)
_cell_measurement_reflns_used    3544
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      19.753
_cell_measurement_theta_min      2.319
_cell_volume                     14788(2)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0963
_diffrn_reflns_av_unetI/netI     0.1765
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            62674
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        21.746
_diffrn_reflns_theta_max         21.746
_diffrn_reflns_theta_min         1.477
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    19.514
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.4999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1197 before and 0.0523 after correction.
The Ratio of minimum to maximum transmission is 0.6713.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.026
_exptl_crystal_description       block
_exptl_crystal_F_000             11784
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.815
_refine_diff_density_min         -1.837
_refine_diff_density_rms         0.391
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2271
_refine_ls_number_reflns         34925
_refine_ls_number_restraints     992
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1702
_refine_ls_R_factor_gt           0.0756
_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^)+(0.0749P)^2^+561.8654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1707
_refine_ls_wR_factor_ref         0.2282
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17324
_reflns_number_total             34925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01282g2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7707959--7707960.cif.'
_cod_original_cell_volume        14788.0(19)
_cod_database_code               7707959
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.127
_shelx_estimated_absorpt_t_min   0.112
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C8-N1
 1.45 with sigma of 0.01
 C1-N2
 1.45 with sigma of 0.01
 C4-N2
 1.45 with sigma of 0.01
 C6-N1
 1.45 with sigma of 0.01
 C8-N1 = N1-C6
 1.45 with sigma of 0.02
 C5-N4 = N4-C2
 1.45 with sigma of 0.02
 C7-N3 = N3-C3
 1.45 with sigma of 0.02
 C8-C6
 2.511 with sigma of 0.04
 C5-C2
 2.511 with sigma of 0.04
 C7-C3
 2.511 with sigma of 0.04
 Yb1-H11A \\sim Yb1-H11B
 with sigma of 0.02
3. Rigid bond restraints
 O77, Yb4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O63, Yb4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O43 \\sim O66 \\sim O114 \\sim O146 \\sim O179: within 5A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 5A
Uanis(O48) \\sim Ueq, Uanis(O77) \\sim Ueq, Uanis(O145) \\sim Ueq, Uanis(O66)
\\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O98) \\sim Ueq,
Uanis(O83) \\sim Ueq, Uanis(O135) \\sim Ueq, Uanis(O184) \\sim Ueq, Uanis(O37)
\\sim Ueq, Uanis(O93) \\sim Ueq, Uanis(O153) \\sim Ueq, Uanis(O157) \\sim Ueq,
Uanis(O53) \\sim Ueq, Uanis(O109) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O169) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O41) \\sim Ueq, Uanis(Na1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O68) \\sim Ueq, Uanis(O63) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O114) \\sim Ueq, Uanis(O147) \\sim Ueq, Uanis(O85) \\sim Ueq, Uanis(O57)
\\sim Ueq, Uanis(O167) \\sim Ueq, Uanis(O127) \\sim Ueq, Uanis(O139) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O90) \\sim Ueq, Uanis(O1)
\\sim Ueq, Uanis(O159) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O84) \\sim Ueq,
Uanis(O50) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6) \\sim Ueq, Uanis(O39) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O62)
\\sim Ueq, Uanis(O138) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O117) \\sim Ueq,
Uanis(O148) \\sim Ueq, Uanis(O76) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O122) \\sim Ueq, Uanis(O159) \\sim Ueq, Uanis(O119) \\sim Ueq, Uanis(O62)
\\sim Ueq, Uanis(O39) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O3) \\sim Ueq, Uanis(O159) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O62)
\\sim Ueq, Uanis(O39) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O26) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O182) \\sim Ueq, Uanis(O34)
\\sim Ueq, Uanis(O105) \\sim Ueq, Uanis(O74) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O34) \\sim Ueq, Uanis(O58) \\sim Ueq, Uanis(O182) \\sim Ueq, Uanis(O4)
\\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O142) \\sim Ueq, Uanis(O29) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O46) \\sim Ueq, Uanis(O81) \\sim Ueq, Uanis(O111) \\sim Ueq, Uanis(O92)
\\sim Ueq, Uanis(O141) \\sim Ueq, Uanis(O107) \\sim Ueq, Uanis(O125) \\sim Ueq,
Uanis(O146) \\sim Ueq, Uanis(O134) \\sim Ueq, Uanis(O79) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O96) \\sim Ueq, Uanis(O174) \\sim Ueq, Uanis(O149) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O182) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O34) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O34) \\sim Ueq, Uanis(O26) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O182) \\sim Ueq, Uanis(O178) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O90) \\sim Ueq, Uanis(O39) \\sim Ueq, Uanis(O126) \\sim Ueq, Uanis(O62)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O159) \\sim Ueq, Uanis(O39) \\sim Ueq, Uanis(O62) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O182) \\sim Ueq, Uanis(O30) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O39) \\sim Ueq, Uanis(O62) \\sim Ueq, Uanis(O182) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(O170) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O130) \\sim Ueq, Uanis(O163) \\sim Ueq, Uanis(O59) \\sim Ueq, Uanis(O78)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O171) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O55) \\sim Ueq, Uanis(O159) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O159) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O112) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O64) \\sim Ueq, Uanis(O94) \\sim Ueq, Uanis(O180) \\sim Ueq, Uanis(O56)
\\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O44) \\sim Ueq,
Uanis(O18) \\sim Ueq, Uanis(O55) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O55) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O137) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O69) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(O40) \\sim Ueq, Uanis(O119) \\sim Ueq, Uanis(O88)
\\sim Ueq, Uanis(O120) \\sim Ueq, Uanis(O90) \\sim Ueq, Uanis(O32) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O36) \\sim Ueq, Uanis(O154) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O5) \\sim Ueq, Uanis(O90) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O132)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O118) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O113) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O152) \\sim Ueq, Uanis(O158) \\sim Ueq, Uanis(O33) \\sim Ueq, Uanis(O124)
\\sim Ueq, Uanis(O186) \\sim Ueq, Uanis(O121) \\sim Ueq, Uanis(O60) \\sim Ueq,
Uanis(O106) \\sim Ueq, Uanis(O50) \\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(O28)
\\sim Ueq, Uanis(O100) \\sim Ueq, Uanis(O80) \\sim Ueq, Uanis(O51) \\sim Ueq,
Uanis(O173) \\sim Ueq, Uanis(O101) \\sim Ueq, Uanis(O123) \\sim Ueq, Uanis(O35)
\\sim Ueq, Uanis(O165) \\sim Ueq, Uanis(O73) \\sim Ueq, Uanis(O45) \\sim Ueq,
Uanis(O175) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O11) \\sim Ueq, Uanis(O45) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O179) \\sim Ueq, Uanis(O143) \\sim Ueq, Uanis(O86) \\sim Ueq, Uanis(O43)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O70) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O117) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O164) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O174) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(N2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C8) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(N2) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.001 and sigma
for terminal atoms of 0.002
Uanis(C5) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(N3) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(N1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O177) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O91) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O131) \\sim Ueq, Uanis(O63) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O82) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O9) \\sim Ueq, Uanis(O102) \\sim Ueq, Uanis(O151) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 W33
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 W29
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 W29, O179
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 W33, O179
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N1, C8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C6, N1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: O171(0.25) N1(0.5) H1A(0.5) H1B(0.5) O85(0.75) C6(0.5) H6A(0.5)
 H6B(0.5) H6C(0.5) C8(0.5) H8A(0.5) H8B(0.5) H8C(0.5) N3(0.5) H3A(0.5) H3B(0.5)
 C3(0.5) H3C(0.5) H3D(0.5) H3E(0.5) C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5) O23(0.5)
 O91(0.5)
7.a Free rotating group:
 O117(H11A,H11B)
7.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N4(H4A,H4B), N2(H2D,H2E), N3(H3A,H3B)
7.c X=CH2 refined with riding coordinates:
 O149(H14A,H14B)
7.d Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E), C4(H4C,H4D,H4E), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C2(H2A,
 H2B,H2C), C5(H5A,H5B,H5C), C3(H3C,H3D,H3E), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              92003
_olex2_submission_special_instructions 'No special instructions were received'