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_7707960
_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
'H24 Na O172 Se6 W44 Yb4,6(C2 H8 N)??40??H2O??,13??Na??'
_chemical_formula_sum            'C12 H152 N6 Na14 O212 Se6 W44 Yb4'
_chemical_formula_weight         13350.57
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   50.919(2)
_cell_length_b                   23.3103(8)
_cell_length_c                   20.2832(8)
_cell_measurement_reflns_used    6058
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.03
_cell_measurement_theta_min      2.18
_cell_volume                     24074.9(16)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1655
_diffrn_reflns_av_unetI/netI     0.1079
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            135589
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.792
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.499
_exptl_absorpt_correction_T_max  0.166
_exptl_absorpt_correction_T_min  0.089
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/4 Bruker AXS Madison WI USA'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.683
_exptl_crystal_description       block
_exptl_crystal_F_000             23424
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.770
_refine_diff_density_min         -2.329
_refine_diff_density_rms         0.468
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1284
_refine_ls_number_reflns         21189
_refine_ls_number_restraints     308
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1190
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0491P)^2^+556.5095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1392
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12584
_reflns_number_total             21189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01282g2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7707959--7707960.cif.'
_cod_original_cell_volume        24074.8(16)
_cod_database_code               7707960
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.127
_shelx_estimated_absorpt_t_min   0.089
_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
 Se2-O20
 1.75 with sigma of 0.01
 O11-Se1
 1.78 with sigma of 0.02
 Se7-O84 = Se7-O87 = Se7-O20
 1.78 with sigma of 0.02
 O87-O20
 2.2 with sigma of 0.2
 N4-C6
 1.45 with sigma of 0.02
 N4-C8
 1.45 with sigma of 0.02
 C2-N2
 1.45 with sigma of 0.02
 N2-C5
 1.45 with sigma of 0.02
 N3-C7 = N3-C3
 1.45 with sigma of 0.02
 N1-C4
 1.5 with sigma of 0.01
 N1-C1
 1.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N1 \\sim C1 \\sim C4: within 5A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 5A
O11 \\sim O20 \\sim O31 \\sim O84 \\sim O87: within 5A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 5A
Uanis(O14) \\sim Ueq, Uanis(O72) \\sim Ueq, Uanis(O41) \\sim Ueq, Uanis(O22)
\\sim Ueq, Uanis(O52) \\sim Ueq, Uanis(O74) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(O19) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Se2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O20) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O66) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O30) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O48) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O87) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O77) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O88) \\sim Ueq, Uanis(O79) \\sim Ueq, Uanis(O83) \\sim Ueq, Uanis(O51)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C1) \\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(O93) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O95) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C6) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(N2) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O47) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O45) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Se3) \\sim Ueq, Uanis(Se5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: W22(0.5) W23(0.5) Se1(0.3) Se2(0.2) Se3(0.2) Se5(0.15) Se7(0.15)
 Na1(0.5) O11(0.3) O20(0.15) O31(0.75) O84(0.15) O87(0.15) O3(0.5) O23(0.5)
 O45(0.25) O47(0.75) O93(0.75) O95(0.75) N1(0.5) H1A(0.5) H1B(0.5) C1(0.5)
 H1C(0.5) H1D(0.5) H1E(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5) N2(0.5) H2A(0.5)
 H2B(0.5) C2(0.5) H2C(0.5) H2D(0.5) H2E(0.5) C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5)
 N3(0.4) H3A(0.4) H3B(0.4) C3(0.4) H3C(0.4) H3D(0.4) H3E(0.4) C7(0.4) H7A(0.4)
 H7B(0.4) H7C(0.4) N4(0.6) H4D(0.6) H4E(0.6) C6(0.6) H6A(0.6) H6B(0.6) H6C(0.6)
 C8(0.6) H8A(0.6) H8B(0.6) H8C(0.6)
5.a Rotating group:
 O80(H80A,H80B)
5.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B), N4(H4D,H4E)
5.c Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E), C4(H4A,H4B,H4C), C2(H2C,H2D,H2E), C5(H5A,H5B,H5C), C3(H3C,
 H3D,H3E), C7(H7A,H7B,H7C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              96024
_olex2_submission_special_instructions 'No special instructions were received'