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_4344379
_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         'H148 Li12 Na8 Ni2 O186 P4 W30'
_chemical_formula_sum            'H148 Li12 Na8 Ni2 O186 P4 W30'
_chemical_formula_weight         9149.17
_chemical_name_common            2014-05-12
_chemical_name_systematic
;
 ?
;
_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_primary     iterative
_audit_creation_date             2014-12-17
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_cell_angle_alpha                75.983(2)
_cell_angle_beta                 81.838(2)
_cell_angle_gamma                61.8110(10)
_cell_formula_units_Z            1
_cell_length_a                   13.2155(15)
_cell_length_b                   13.380(2)
_cell_length_c                   25.206(4)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      29.690
_cell_measurement_theta_min      2.454
_cell_volume                     3809.4(9)
_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 0.998
_diffrn_measured_fraction_theta_max 0.993
_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  0.0508
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            64611
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.727
_diffrn_reflns_theta_min         1.763
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30
_diffrn_source_voltage           45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.992
_exptl_absorpt_correction_T_max  0.1281
_exptl_absorpt_correction_T_min  0.0492
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1010 before and 0.0552 after correction.
The Ratio of minimum to maximum transmission is 0.3841.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    3.988
_exptl_crystal_description       prism
_exptl_crystal_F_000             4096
_exptl_crystal_recrystallization_method
'The material was recrystallised from water by slow evaporation'
_exptl_crystal_size_max          0.335
_exptl_crystal_size_mid          0.282
_exptl_crystal_size_min          0.228
_refine_diff_density_max         3.840
_refine_diff_density_min         -3.682
_refine_diff_density_rms         0.437
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1029
_refine_ls_number_reflns         21521
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+106.7675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1273
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15936
_reflns_number_total             21521
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01935_si_002.cif
_cod_data_source_block           20140512
_cod_depositor_comments
'Adding full bibliography for 4344379--4344380.cif.'
_cod_database_code               4344379
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(Li2) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(O24W) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(O13W) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(O3W) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(W2') = Uanis(W1') = Uanis(W3')
Uanis(W13) = Uanis(W13')
Uanis(W15) = Uanis(W15')
Uanis(W12') = Uanis(W12)
Uanis(W10) = Uanis(W10')
Uanis(W11) = Uanis(W11')
Uanis(W14') = Uanis(W14)
Uiso(Na3C) = Uiso(Na3B)
Uiso(Na3A) = Uiso(Na3C)
Uiso(Na3A) = Uiso(Na3B)
Uanis(Na1B) = Uanis(Na1A)
Uanis(O5) = Uanis(W2')
Uanis(O4) = Uanis(W3')
Uanis(O3) = Uanis(W1')
Uanis(O29W) = Uanis(O29W)
Uanis(O29') = Uanis(O29W)
2. Rigid body (RIGU) restrains
 Na1B, Na1A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O1, P1, Ni1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O21, O25, O29, O1, P1
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
 O43, Ni1, W11
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O46, W10
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O33, W15
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O36, W13
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O12W, Li3
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O10W, Li3
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Li2, O29W
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O41, W12
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O12W, Li3
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Others
 Sof(W1)=Sof(W2)=Sof(W3)=1-FVAR(1)
 Sof(W1')=Sof(W3')=Sof(W2')=FVAR(1)
 Sof(W15)=1-FVAR(2)
 Sof(W13')=Sof(W15')=FVAR(2)
 Sof(W10)=Sof(W11)=Sof(W12)=Sof(W13)=Sof(W14)=1-FVAR(3)
 Sof(W11')=Sof(W14')=Sof(W12')=Sof(W10')=FVAR(3)
 Sof(O29')=1-FVAR(4)
 Sof(O29W)=FVAR(4)
 Fixed Sof: Na3A(0.33333) Na1B(0.5) Na1A(0.5) Na3B(0.33333) O13W(0.5)
 Na3C(0.33333)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop with paratone oil'
_olex2_submission_original_sample_id 2014-05-12
_olex2_submission_special_instructions 'No special instructions were received'