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_7030077
_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            'B6 Na14 Ni8 O122 Si2 W18'
_chemical_formula_weight         6173.5
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   21.8496(16)
_cell_length_b                   21.8496(16)
_cell_length_c                   44.606(4)
_cell_measurement_reflns_used    9205
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.09
_cell_measurement_theta_min      1.74
_cell_volume                     18442(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1378
_diffrn_reflns_av_unetI/netI     0.0691
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            95651
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    18.124
_exptl_absorpt_correction_T_max  0.095
_exptl_absorpt_correction_T_min  0.074
_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    3.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             15722.1
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_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. Squeeze results were attached as above. Overall consideration 
 the TG, elemental analysis,and crystallography, another fourteen water 
 molecules were included in the final molecules. 
;
_refine_diff_density_max         3.313
_refine_diff_density_min         -1.773
_refine_diff_density_rms         0.336
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_matrix_type           full
_refine_ls_number_parameters     684
_refine_ls_number_reflns         11057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+715.8359P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1478
_reflns_number_gt                8606
_reflns_number_total             11057
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51201k.cif
_cod_data_source_block           1
_cod_original_cell_volume        18442(2)
_cod_original_sg_symbol_H-M      P63/m
_cod_database_code               7030077