Poly(polyoxometalate)s assembled by {Ni6PW9} units: from ring-shaped Ni24-tetramers to rod-shaped Ni40-octamers
Ling Huang; Jie Zhang; Lin Cheng; Guo-Yu Yang; Chem.Commun. 48 (2012) 9658–; doi:10.1039/c2cc34332k

data_7108344
_publ_section_title
;
 Poly(polyoxometalate)s assembled by {Ni6PW9} units: from ring-shaped
 Ni24-tetramers to rod-shaped Ni40-octamers
;
_journal_name_full               Chem.Commun.
_journal_page_first              9658
_journal_paper_doi               10.1039/c2cc34332k
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C50 H210 N28 Ni25 O178 P4 W36'
_chemical_formula_weight         12262.69
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.402(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   20.518(3)
_cell_length_b                   23.518(3)
_cell_length_c                   27.721(5)
_cell_measurement_reflns_used    36919
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4855
_cell_measurement_theta_min      2.0335
_cell_volume                     12454(3)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  SCXMini
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0822
_diffrn_reflns_av_sigmaI/netI    0.0765
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            107016
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    18.509
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             11108
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         4.185
_refine_diff_density_min         -2.378
_refine_diff_density_rms         0.485
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1384
_refine_ls_number_reflns         28481
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0863
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0571P)^2^+800.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1896
_refine_ls_wR_factor_ref         0.2008
_reflns_number_gt                26117
_reflns_number_total             28481
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc34332k.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7108344