Borate-templated self-assembly of multinuclear nickel(II)-containing POMs.
Li, Shujun; Liu, Shuxia; Tang, Qun; Liu, Yiwei; He, Danfeng; Wang, Shengtian; Shi, Zhan; Dalton transactions (Cambridge, England : 2003) 42 (2013) 13319–13322; doi:10.1039/c3dt51201k

data_7030078
_publ_section_title
;
 Borate-templated self-assembly of multinuclear nickel(II)-containing
 POMs.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13319
_journal_page_last               13322
_journal_paper_doi               10.1039/c3dt51201k
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'B3 Na20 Ni12 O167 P Si3 W27'
_chemical_formula_weight         8947.3
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.983(2)
_cell_angle_beta                 87.260(2)
_cell_angle_gamma                63.067(2)
_cell_formula_units_Z            2
_cell_length_a                   20.919(2)
_cell_length_b                   22.998(3)
_cell_length_c                   23.393(3)
_cell_measurement_reflns_used    4310
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.020
_cell_measurement_theta_min      1.30
_cell_volume                     9419(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SMART'
_computing_publication_material  'Bruker SMART'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean '100x100 microns'
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0928
_diffrn_reflns_av_unetI/netI     0.2449
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            55382
_diffrn_reflns_theta_full        27.02
_diffrn_reflns_theta_max         27.02
_diffrn_reflns_theta_min         1.30
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    17.755
_exptl_absorpt_correction_T_max  0.202
_exptl_absorpt_correction_T_min  0.020
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       square
_exptl_crystal_F_000             7704.9
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
 Platon Squeeze procedure was used to estimate and remove the solvent area 
 contents which were attributed to partially unseen solvent water molecules
 and counterions.The resulting new HKL file was not applied for further 
 refine. Squeeze results were attached as above. Overall consideration 
 the TG, elemental analysis,and crystallography, another 12.5 water 
 molecules were included in the final molecules. 
 
 Residual electron density peaks were observed close to the 
 heavy metal atoms W. No further disorder models were attempted 
 as the reflection data quality was very limited. The POM cluster
 was generally well defined with clear heavy metal atom sites and
 terminal and bridging oxo sites.
;
_refine_diff_density_max         3.496
_refine_diff_density_min         -4.255
_refine_diff_density_rms         0.573
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1869
_refine_ls_number_reflns         39748
_refine_ls_number_restraints     474
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.1962
_refine_ls_R_factor_gt           0.0833
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0680P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1767
_refine_ls_wR_factor_ref         0.2250
_reflns_number_gt                18373
_reflns_number_total             39748
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51201k.cif
_cod_data_source_block           2
_cod_original_cell_volume        9419.2(18)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7030078