Two extended structures constructed from sandwich-type polyoxometalates functionalized by organic amines
Zhang, Zhiming; Liu, Jia; Wang, Enbo; Qin, Chao; Li, Yangguang; Qi, Yanfei; Wang, Xinlong; Dalton Transactions  (2008) 463–468; doi:10.1039/b712903c

data_7003130
_publ_section_title
;
 Two extended structures constructed from sandwich-type
 polyoxometalates functionalized by organic amines
;
_journal_issue                   4
_journal_name_full               'Dalton Transactions'
_journal_page_first              463
_journal_page_last               468
_journal_paper_doi               10.1039/b712903c
_journal_year                    2008
_chemical_formula_sum            'C24 H86 N8 Na2 Ni4 O75 P2 W18'
_chemical_formula_weight         5339.07
_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_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                118.00(3)
_cell_angle_beta                 97.20(3)
_cell_angle_gamma                105.12(3)
_cell_formula_units_Z            1
_cell_length_a                   11.727(2)
_cell_length_b                   15.710(3)
_cell_length_c                   16.103(3)
_cell_measurement_reflns_used    8350
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      3.00
_cell_volume                     2419.5(14)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.01
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku RAXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_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  0.1029
_diffrn_reflns_av_sigmaI/netI    0.1437
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18651
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    22.197
_exptl_absorpt_correction_T_max  0.009
_exptl_absorpt_correction_T_min  0.003
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'
_exptl_crystal_colour            'rellow green'
_exptl_crystal_density_diffrn    3.664
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2382
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.571
_refine_diff_density_min         -2.576
_refine_diff_density_rms         0.485
_refine_ls_extinction_coef       0.00081(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         8350
_refine_ls_number_restraints     226
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1406
_refine_ls_wR_factor_ref         0.1579
_reflns_number_gt                5623
_reflns_number_total             8350
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b712903c.txt
_cod_data_source_block           2
_cod_original_cell_volume        2419.5(8)
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               7003130