Utilizing the adaptive precursor [As<sub>2</sub>W<sub>19</sub>O<sub>67</sub>(H<sub>2</sub>O)]<sup>14-</sup> to support three hexanuclear lanthanoid-based tungstoarsenate dimers.
Li, Huafeng; Wu, Hechen; Wan, Rong; Wang, Yuan; Ma, Pengtao; Li, Suzhi; Wang, Jingping; Niu, Jingyang; Dalton transactions (Cambridge, England : 2003) 48 (2019) 2813–2821; doi:10.1039/c8dt04944k

data_7048948
_publ_section_title
;
 Utilizing the adaptive precursor
 [As<sub>2</sub>W<sub>19</sub>O<sub>67</sub>(H<sub>2</sub>O)]<sup>14-</sup>
 to support three hexanuclear lanthanoid-based tungstoarsenate dimers.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2813
_journal_page_last               2821
_journal_paper_doi               10.1039/c8dt04944k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C8 H4 As4 Dy6 K15 O180.5 W38, 8.5(O)'
_chemical_formula_sum            'C8 H4 As4 Dy6 K15 O189 W38'
_chemical_formula_weight         11971.59
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc124x59
_audit_creation_date             2019-01-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-14 deposited with the CCDC.
2019-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                91.6410(10)
_cell_angle_beta                 100.0280(10)
_cell_angle_gamma                108.4640(10)
_cell_formula_units_Z            2
_cell_length_a                   19.5603(8)
_cell_length_b                   22.5308(9)
_cell_length_c                   26.0965(11)
_cell_measurement_reflns_used    9960
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.49
_cell_measurement_theta_min      2.24
_cell_volume                     10699.0(8)
_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  '2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'ShelXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0374
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            56635
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         1.737
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.405
_exptl_absorpt_correction_T_max  0.0137
_exptl_absorpt_correction_T_min  0.0015
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.716
_exptl_crystal_description       block
_exptl_crystal_F_000             10378
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.424
_refine_diff_density_min         -1.965
_refine_diff_density_rms         0.432
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2276
_refine_ls_number_reflns         37889
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0571
_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^)+(0.1013P)^2^+15.1993P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1543
_refine_ls_wR_factor_ref         0.1682
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28895
_reflns_number_total             37889
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04944k2.cif
_cod_data_source_block           987820
_cod_depositor_comments
'Adding full bibliography for 7048946--7048948.cif.'
_cod_database_code               7048948
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.102
_shelx_estimated_absorpt_t_min   0.042
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 C1, O71
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
O71 \\sim C1: within 1.5A with sigma of 0.01 and sigma for terminal atoms of
0.02
K9 \\sim O20: within 3A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(K13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: K11(0.75) K12(0.75) K13(0.75) K14(0.75) K15(0.5) K16(0.5) K17(0.5)
 K18(0.5) O21W(0.5) O34W(0.5) O33W(0.5) O17W(0.5)
5.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7)
;
_shelx_res_checksum              26150
_shelx_fab_checksum              23991
_olex2_submission_special_instructions 'No special instructions were received'