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_7705892
_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         '0.11(Ni2 O76 Sb2 W20), 1.26(O)'
_chemical_formula_sum            'Ni0.21 O9.26 Sb0.21 W2.11'
_chemical_formula_weight         573.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_primary     iterative
_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                 113.239(9)
_cell_angle_gamma                90
_cell_formula_units_Z            19
_cell_length_a                   17.8033(14)
_cell_length_b                   18.5672(16)
_cell_length_c                   14.1660(12)
_cell_measurement_reflns_used    1846
_cell_measurement_temperature    178.3(6)
_cell_measurement_theta_max      28.2430
_cell_measurement_theta_min      3.3140
_cell_volume                     4302.8(7)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      178.3(6)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
  1 omega  -99.00   38.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.0453    0.0000  150.0000 137

  2 omega  -64.00    7.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.0453  -57.0000   90.0000 71

  3 omega   59.00   84.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       24.2953  178.0000  150.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0433422000
_diffrn_orient_matrix_UB_12      0.0013823000
_diffrn_orient_matrix_UB_13      0.0216733000
_diffrn_orient_matrix_UB_21      -0.0015486000
_diffrn_orient_matrix_UB_22      0.0359641000
_diffrn_orient_matrix_UB_23      0.0161166000
_diffrn_orient_matrix_UB_31      0.0004313000
_diffrn_orient_matrix_UB_32      -0.0129050000
_diffrn_orient_matrix_UB_33      0.0472908000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0758
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7261
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.078
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    27.761
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39064
_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            yellow-green
_exptl_crystal_density_diffrn    4.203
_exptl_crystal_description       block
_exptl_crystal_F_000             4684
_refine_diff_density_max         3.165
_refine_diff_density_min         -6.826
_refine_diff_density_rms         0.502
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         3883
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0678
_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^)+(0.0755P)^2^+462.1729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1689
_refine_ls_wR_factor_ref         0.1788
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3227
_reflns_number_total             3883
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02409k2.cif
_cod_data_source_block           exp_14837
_cod_database_code               7705892
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 98.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O15) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O14)
\\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O12) \\sim Ueq,
Uanis(O10) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O9) \\sim
Ueq, Uanis(O4AA) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O16) \\sim Ueq,
Uanis(O2W) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O17)
\\sim Ueq, Uanis(O1W) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O3AA) \\sim Ueq,
Uanis(O19) \\sim Ueq, Uanis(O0AA) \\sim Ueq, Uanis(O1AA) \\sim Ueq, Uanis(O2AA)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
2. Others
 Fixed Sof: O2AA(0.5)
;
_shelx_res_checksum              6390
_shelx_fab_checksum              1504
_olex2_date_sample_data_collection 2016-09-13
_olex2_submission_special_instructions 'No special instructions were received'