Syntheses, Structural Characterization, and Catalytic Properties of Di- and Trinickel Polyoxometalates.
Guo, Weiwei; Lv, Hongjin; Bacsa, John; Gao, Yuanzhe; Lee, Je Seong; Hill, Craig L.; Inorganic chemistry 55 (2016) 461–466; doi:10.1021/acs.inorgchem.5b01935

data_4344380
_publ_section_title
;
 Syntheses, Structural Characterization, and Catalytic Properties of Di-
 and Trinickel Polyoxometalates.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              461
_journal_page_last               466
_journal_paper_doi               10.1021/acs.inorgchem.5b01935
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'H9 Ni3 O65 P2 W15.89, 0.11(W)'
_chemical_formula_sum            'H101 Li5 Na5 Ni3 O111 P2 W16'
_chemical_formula_weight         5207.12
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-12-10
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.364(5)
_cell_length_b                   24.299(5)
_cell_length_c                   28.863(6)
_cell_measurement_reflns_used    9666
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      30.376
_cell_measurement_theta_min      2.188
_cell_volume                     17087(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2014.1-1 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            237802
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.479
_diffrn_reflns_theta_min         1.378
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30
_diffrn_source_voltage           45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.304
_exptl_absorpt_correction_T_max  0.2267
_exptl_absorpt_correction_T_min  0.0161
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.0986 before and 0.0673 after correction.
The Ratio of minimum to maximum transmission is 0.0710.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    4.048
_exptl_crystal_description       prism
_exptl_crystal_F_000             18856
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.311
_exptl_crystal_size_min          0.124
_refine_diff_density_max         3.933
_refine_diff_density_min         -4.408
_refine_diff_density_rms         0.508
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     792
_refine_ls_number_reflns         25653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0547
_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^)+(0.0967P)^2^+253.8076P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1678
_refine_ls_wR_factor_ref         0.1793
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19478
_reflns_number_total             25653
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01935_si_003.cif
_cod_data_source_block           2014-5-22-5
_cod_depositor_comments
'Adding full bibliography for 4344379--4344380.cif.'
_cod_database_code               4344380
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(W7) = Uanis(W7')
Uanis(W2B) = Uanis(W2)
Uanis(W3B) = Uanis(W3)
Uanis(W1B) = Uanis(W1)
3. Others
 Sof(W1B)=Sof(W3B)=Sof(W2B)=1-FVAR(1)
 Sof(W1)=Sof(W2)=Sof(W3)=FVAR(1)
 Sof(W7')=1-FVAR(2)
 Sof(W7)=FVAR(2)
4.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB)
4.b Ternary CH refined with riding coordinates:
 O34(H34), O35(H35), O38(H38)
;
_shelx_fab_checksum              39164
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_special_instructions 'No special instructions were received'