Ionic strength effect on regulating the synthetic assembly of polyoxometalate clusters with slow magnetic relaxation behavior.
Cai, Jing; Ye, Run; Liu, Xinhao; Guo, Leilei; Qiao, Xinrong; Dalton transactions (Cambridge, England : 2003) 49 (2020) 16954–16961; doi:10.1039/d0dt02409k

data_7705893
_publ_section_title
;
 Ionic strength effect on regulating the synthetic assembly of
 polyoxometalate clusters with slow magnetic relaxation behavior.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16954
_journal_page_last               16961
_journal_paper_doi               10.1039/d0dt02409k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'Dy3 K4 Na4.75 O126.58 Sb4 W30, 11.75(O)'
_chemical_formula_sum            'Dy3 K4 Na4.75 O138.33 Sb3 W31'
_chemical_formula_weight         9031.04
_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_primary     dual
_audit_creation_date             2020-06-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-01 deposited with the CCDC.	2020-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.193(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.159(3)
_cell_length_b                   18.5597(7)
_cell_length_c                   48.357(3)
_cell_measurement_reflns_used    3672
_cell_measurement_temperature    191(2)
_cell_measurement_theta_max      24.8130
_cell_measurement_theta_min      3.3690
_cell_volume                     28783(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      191(2)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -66.00   14.25   0.7500   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7912  -77.0000   30.0000 107

  2 omega  -72.00   53.25   0.7500   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7912   19.0000  -60.0000 167

  3 omega   25.00   53.50   0.7500   50.0000
omega____ theta____ kappa____ phi______ frames
    -       19.0412  -99.0000 -180.0000 38
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0045420000
_diffrn_orient_matrix_UB_12      0.0043523000
_diffrn_orient_matrix_UB_13      0.0128922000
_diffrn_orient_matrix_UB_21      -0.0009364000
_diffrn_orient_matrix_UB_22      -0.0379916000
_diffrn_orient_matrix_UB_23      0.0012823000
_diffrn_orient_matrix_UB_31      0.0216196000
_diffrn_orient_matrix_UB_32      -0.0007927000
_diffrn_orient_matrix_UB_33      0.0095323000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1064
_diffrn_reflns_av_unetI/netI     0.1780
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            51877
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.853
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    26.985
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.168
_exptl_crystal_description       rodlike
_exptl_crystal_F_000             31039
_refine_diff_density_max         7.824
_refine_diff_density_min         -4.386
_refine_diff_density_rms         0.621
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1789
_refine_ls_number_reflns         25278
_refine_ls_number_restraints     961
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1583
_refine_ls_R_factor_gt           0.1059
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+6694.0288P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2022
_refine_ls_wR_factor_ref         0.2298
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16249
_reflns_number_total             25278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02409k2.cif
_cod_data_source_block           exp_14759
_cod_original_cell_volume        28784(4)
_cod_database_code               7705893
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Restrained distances
 K0AA-O0AA
 2.8 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(Na3) \\sim Ueq, Uanis(Na1) \\sim Ueq, Uanis(Na0A) \\sim Ueq, Uanis(K12)
\\sim Ueq, Uanis(K0A) \\sim Ueq, Uanis(Na2) \\sim Ueq, Uanis(Na6) \\sim Ueq,
Uanis(Na7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Na4) \\sim Ueq, Uanis(K5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O49) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(O87) \\sim Ueq, Uanis(O0AA)
\\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O77) \\sim Ueq,
Uanis(O96) \\sim Ueq, Uanis(O58) \\sim Ueq, Uanis(O128) \\sim Ueq, Uanis(O55)
\\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(O105) \\sim Ueq, Uanis(O116) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O117)
\\sim Ueq, Uanis(O88) \\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(O108) \\sim Ueq,
Uanis(O109) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O57) \\sim Ueq, Uanis(O110)
\\sim Ueq, Uanis(O39) \\sim Ueq, Uanis(O102) \\sim Ueq, Uanis(O26) \\sim Ueq,
Uanis(O98) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O71) \\sim Ueq, Uanis(O92)
\\sim Ueq, Uanis(O44) \\sim Ueq, Uanis(O96) \\sim Ueq, Uanis(O170) \\sim Ueq,
Uanis(O97) \\sim Ueq, Uanis(O104) \\sim Ueq, Uanis(O85) \\sim Ueq, Uanis(O51)
\\sim Ueq, Uanis(O58) \\sim Ueq, Uanis(O143) \\sim Ueq, Uanis(O54) \\sim Ueq,
Uanis(O81) \\sim Ueq, Uanis(O120) \\sim Ueq, Uanis(O90) \\sim Ueq, Uanis(O162)
\\sim Ueq, Uanis(O50) \\sim Ueq, Uanis(O74) \\sim Ueq, Uanis(O115) \\sim Ueq,
Uanis(O118) \\sim Ueq, Uanis(O29) \\sim Ueq, Uanis(O121) \\sim Ueq, Uanis(O41)
\\sim Ueq, Uanis(O113) \\sim Ueq, Uanis(O48) \\sim Ueq, Uanis(O30) \\sim Ueq,
Uanis(O27) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O77) \\sim Ueq, Uanis(O87)
\\sim Ueq, Uanis(O99) \\sim Ueq, Uanis(O43) \\sim Ueq, Uanis(O32) \\sim Ueq,
Uanis(O4) \\sim Ueq, Uanis(O142) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O107)
\\sim Ueq, Uanis(O64) \\sim Ueq, Uanis(O55) \\sim Ueq, Uanis(O18) \\sim Ueq,
Uanis(O72) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O78) \\sim Ueq, Uanis(O112)
\\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O36) \\sim Ueq,
Uanis(O62) \\sim Ueq, Uanis(O59) \\sim Ueq, Uanis(O75) \\sim Ueq, Uanis(O61)
\\sim Ueq, Uanis(O159) \\sim Ueq, Uanis(O56) \\sim Ueq, Uanis(O52) \\sim Ueq,
Uanis(O128) \\sim Ueq, Uanis(O91) \\sim Ueq, Uanis(O38) \\sim Ueq, Uanis(O70)
\\sim Ueq, Uanis(O80) \\sim Ueq, Uanis(O53) \\sim Ueq, Uanis(O14) \\sim Ueq,
Uanis(O63) \\sim Ueq, Uanis(O76) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O1)
\\sim Ueq, Uanis(O123) \\sim Ueq, Uanis(O94) \\sim Ueq, Uanis(O47) \\sim Ueq,
Uanis(O114) \\sim Ueq, Uanis(O103) \\sim Ueq, Uanis(O67) \\sim Ueq, Uanis(O4AA)
\\sim Ueq, Uanis(O66) \\sim Ueq, Uanis(O45) \\sim Ueq, Uanis(O5) \\sim Ueq,
Uanis(O106) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O31)
\\sim Ueq, Uanis(O160) \\sim Ueq, Uanis(O83) \\sim Ueq, Uanis(O28) \\sim Ueq,
Uanis(O60) \\sim Ueq, Uanis(O40) \\sim Ueq, Uanis(O42) \\sim Ueq, Uanis(O65)
\\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O34) \\sim Ueq, Uanis(O111) \\sim Ueq,
Uanis(O49) \\sim Ueq, Uanis(O82) \\sim Ueq, Uanis(O93) \\sim Ueq, Uanis(O68)
\\sim Ueq, Uanis(O95) \\sim Ueq, Uanis(O86) \\sim Ueq, Uanis(O19) \\sim Ueq,
Uanis(O69) \\sim Ueq, Uanis(O35) \\sim Ueq, Uanis(O89) \\sim Ueq, Uanis(O10)
\\sim Ueq, Uanis(O100) \\sim Ueq, Uanis(O126) \\sim Ueq, Uanis(O16) \\sim Ueq,
Uanis(O124) \\sim Ueq, Uanis(O165) \\sim Ueq, Uanis(O145) \\sim Ueq, Uanis(O11)
\\sim Ueq, Uanis(O149) \\sim Ueq, Uanis(O133) \\sim Ueq, Uanis(O154) \\sim Ueq,
Uanis(O122) \\sim Ueq, Uanis(O130) \\sim Ueq, Uanis(O125) \\sim Ueq,
Uanis(O139) \\sim Ueq, Uanis(O138) \\sim Ueq, Uanis(O129) \\sim Ueq,
Uanis(O141) \\sim Ueq, Uanis(O167) \\sim Ueq, Uanis(O157) \\sim Ueq,
Uanis(O156) \\sim Ueq, Uanis(O136) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O131)
\\sim Ueq, Uanis(O135) \\sim Ueq, Uanis(O153) \\sim Ueq, Uanis(O163) \\sim Ueq,
Uanis(O158) \\sim Ueq, Uanis(O33) \\sim Ueq, Uanis(O148) \\sim Ueq, Uanis(O155)
\\sim Ueq, Uanis(O79) \\sim Ueq, Uanis(O164) \\sim Ueq, Uanis(O166) \\sim Ueq,
Uanis(O0AA) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: Na1(0.75) K12(0.5) Na6(0.75) O35(0.5) O100(0.5) O126(0.5)
 Na2(0.75) Na7(0.5) O165(0.5) O11(0.5) O154(0.5) O130(0.5) O129(0.75) O141(0.5)
 Na0A(0.5) O167(0.75) O157(0.5) O156(0.5) O136(0.5) O15(0.5) O131(0.5)
 O135(0.5) O153(0.5) Na3(0.5) O158(0.5) O33(0.5) O148(0.5) O155(0.5) O164(0.5)
 O166(0.5) O0AA(0.33333)
;
_shelx_res_checksum              29926
_shelx_fab_checksum              59073
_olex2_date_sample_data_collection 2016-09-06
_olex2_submission_special_instructions 'No special instructions were received'