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_7705891
_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 K5 Na5.33 Ni O130.69 Sb3 W30, 9.08(O)'
_chemical_formula_sum            'Dy3 K5 Na5.34 Ni O139.78 Sb3 W30'
_chemical_formula_weight         8981.59
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_primary     direct
_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                93.078(2)
_cell_angle_beta                 99.426(2)
_cell_angle_gamma                116.645(3)
_cell_formula_units_Z            2
_cell_length_a                   18.2445(6)
_cell_length_b                   19.9956(7)
_cell_length_c                   24.4742(6)
_cell_measurement_reflns_used    11630
_cell_measurement_temperature    186(2)
_cell_measurement_theta_max      26.5810
_cell_measurement_theta_min      3.3040
_cell_volume                     7790.2(5)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      186(2)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -78.00   15.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7912  -77.0000  -90.0000 93

  2 omega  -37.00   53.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7912   57.0000  150.0000 90

  3 omega  -40.00   55.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7912   77.0000   30.0000 95

  4 omega    4.00   64.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1975  -99.0000 -150.0000 60

  5 omega    1.00   58.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1975  -99.0000   90.0000 57

  6 omega   54.00   87.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1975   57.0000    0.0000 33

  7 omega    0.00   31.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1975  -38.0000    0.0000 31

  8 omega    3.00   39.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1975  -57.0000 -120.0000 36

  9 omega   75.00  100.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1975 -178.0000 -120.0000 25

 10 omega   45.00   74.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1975   57.0000  -30.0000 29

 11 omega  -29.00   -2.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1975  -57.0000  -60.0000 27

 12 omega  -52.00  -21.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1975  -38.0000    0.0000 31
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0056848000
_diffrn_orient_matrix_UB_12      0.0308076000
_diffrn_orient_matrix_UB_13      -0.0089965000
_diffrn_orient_matrix_UB_21      0.0409116000
_diffrn_orient_matrix_UB_22      0.0166094000
_diffrn_orient_matrix_UB_23      -0.0056615000
_diffrn_orient_matrix_UB_31      -0.0165409000
_diffrn_orient_matrix_UB_32      -0.0195848000
_diffrn_orient_matrix_UB_33      -0.0277204000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1071
_diffrn_reflns_av_unetI/netI     0.1570
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            69309
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.929
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    24.339
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24871
_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            green
_exptl_crystal_density_diffrn    3.829
_exptl_crystal_description       block
_exptl_crystal_F_000             7742
_refine_diff_density_max         4.277
_refine_diff_density_min         -3.003
_refine_diff_density_rms         0.542
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1784
_refine_ls_number_reflns         27383
_refine_ls_number_restraints     918
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.1293
_refine_ls_R_factor_gt           0.0832
_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^)+(0.1033P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1928
_refine_ls_wR_factor_ref         0.2263
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16781
_reflns_number_total             27383
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02409k2.cif
_cod_data_source_block           exp_14495
_cod_database_code               7705891
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(Na14) \\sim Ueq, Uanis(Na3) \\sim Ueq, Uanis(Na2) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O30) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O111) \\sim Ueq, Uanis(O69)
\\sim Ueq, Uanis(O112) \\sim Ueq, Uanis(O146) \\sim Ueq, Uanis(O84) \\sim Ueq,
Uanis(O89) \\sim Ueq, Uanis(O48) \\sim Ueq, Uanis(O124) \\sim Ueq, Uanis(O44)
\\sim Ueq, Uanis(O34) \\sim Ueq, Uanis(O51) \\sim Ueq, Uanis(O81) \\sim Ueq,
Uanis(O19) \\sim Ueq, Uanis(O117) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O90)
\\sim Ueq, Uanis(O70) \\sim Ueq, Uanis(O118) \\sim Ueq, Uanis(O72) \\sim Ueq,
Uanis(O52) \\sim Ueq, Uanis(O68) \\sim Ueq, Uanis(O125) \\sim Ueq, Uanis(O119)
\\sim Ueq, Uanis(O113) \\sim Ueq, Uanis(O45) \\sim Ueq, Uanis(O87) \\sim Ueq,
Uanis(O33) \\sim Ueq, Uanis(O42) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O147)
\\sim Ueq, Uanis(O122) \\sim Ueq, Uanis(O110) \\sim Ueq, Uanis(O62) \\sim Ueq,
Uanis(O107) \\sim Ueq, Uanis(O57) \\sim Ueq, Uanis(O38) \\sim Ueq, Uanis(O126)
\\sim Ueq, Uanis(O116) \\sim Ueq, Uanis(O139) \\sim Ueq, Uanis(O2) \\sim Ueq,
Uanis(O95) \\sim Ueq, Uanis(O71) \\sim Ueq, Uanis(O105) \\sim Ueq, Uanis(O141)
\\sim Ueq, Uanis(O114) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O39) \\sim Ueq,
Uanis(O94) \\sim Ueq, Uanis(O67) \\sim Ueq, Uanis(O55) \\sim Ueq, Uanis(O36)
\\sim Ueq, Uanis(O108) \\sim Ueq, Uanis(O134) \\sim Ueq, Uanis(O123) \\sim Ueq,
Uanis(O65) \\sim Ueq, Uanis(O60) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O101)
\\sim Ueq, Uanis(O63) \\sim Ueq, Uanis(O58) \\sim Ueq, Uanis(O74) \\sim Ueq,
Uanis(O106) \\sim Ueq, Uanis(O66) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O49)
\\sim Ueq, Uanis(O86) \\sim Ueq, Uanis(O54) \\sim Ueq, Uanis(O80) \\sim Ueq,
Uanis(O14) \\sim Ueq, Uanis(O40) \\sim Ueq, Uanis(O82) \\sim Ueq, Uanis(O91)
\\sim Ueq, Uanis(O31) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O78) \\sim Ueq,
Uanis(O56) \\sim Ueq, Uanis(O115) \\sim Ueq, Uanis(O92) \\sim Ueq, Uanis(O59)
\\sim Ueq, Uanis(O35) \\sim Ueq, Uanis(O85) \\sim Ueq, Uanis(O53) \\sim Ueq,
Uanis(O127) \\sim Ueq, Uanis(O75) \\sim Ueq, Uanis(O47) \\sim Ueq, Uanis(O77)
\\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O50) \\sim Ueq,
Uanis(O28) \\sim Ueq, Uanis(O79) \\sim Ueq, Uanis(O43) \\sim Ueq, Uanis(O96)
\\sim Ueq, Uanis(O73) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O102) \\sim Ueq,
Uanis(O29) \\sim Ueq, Uanis(O88) \\sim Ueq, Uanis(O103) \\sim Ueq, Uanis(O76)
\\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O41) \\sim Ueq, Uanis(O6) \\sim Ueq,
Uanis(O16) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O7)
\\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O131) \\sim Ueq, Uanis(O21) \\sim Ueq,
Uanis(O8) \\sim Ueq, Uanis(O37) \\sim Ueq, Uanis(O100) \\sim Ueq, Uanis(O64)
\\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(O99) \\sim Ueq, Uanis(O24) \\sim Ueq,
Uanis(O25) \\sim Ueq, Uanis(O13W) \\sim Ueq, Uanis(O137) \\sim Ueq, Uanis(O135)
\\sim Ueq, Uanis(O98) \\sim Ueq, Uanis(O121) \\sim Ueq, Uanis(O142) \\sim Ueq,
Uanis(O128) \\sim Ueq, Uanis(O130) \\sim Ueq, Uanis(O109) \\sim Ueq,
Uanis(O133) \\sim Ueq, Uanis(O61) \\sim Ueq, Uanis(O129) \\sim Ueq, Uanis(O120)
\\sim Ueq, Uanis(O46) \\sim Ueq, Uanis(O93) \\sim Ueq, Uanis(O20W) \\sim Ueq,
Uanis(O104) \\sim Ueq, Uanis(O145) \\sim Ueq, Uanis(O32) \\sim Ueq, Uanis(O0DA)
\\sim Ueq, Uanis(O8CA) \\sim Ueq, Uanis(O143) \\sim Ueq, Uanis(O140) \\sim Ueq,
Uanis(O2Y) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O132) \\sim Ueq, Uanis(O97)
\\sim Ueq, Uanis(O136) \\sim Ueq, Uanis(O9BA) \\sim Ueq, Uanis(O4BA) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O129) \\sim Ueq, Uanis(O20W) \\sim Ueq, Uanis(O104) \\sim Ueq,
Uanis(O145) \\sim Ueq, Uanis(O13W) \\sim Ueq, Uanis(O0DA) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.002
2. Others
 Fixed Sof: O13W(0.5) O133(0.75) O61(0.5) O129(0.5) O120(0.5) O46(0.5)
 O93(0.5) O20W(0.5) O104(0.5) O145(0.5) Na14(0.33333) O0DA(0.5) O8CA(0.5)
 O143(0.5) O140(0.5) O23(0.5) O132(0.5) O97(0.5) O136(0.5) O9BA(0.33333)
 O4BA(0.5)
;
_shelx_res_checksum              89913
_shelx_fab_checksum              17337
_olex2_date_sample_data_collection 2016-08-16
_olex2_submission_special_instructions 'No special instructions were received'