Three novel supramolecular hybrid compounds based on keggin polytungstates
Xiao, Li-Na; Wang, Yan; Pan, Cheng-Ling; Xu, Jia-Ning; Wang, Tie-Gang; Ding, Hong; Gao, Zhong-Min; Zheng, Da-Fang; Cui, Xiao-Bing; Xu, Ji-Qing; CrystEngComm 13 (2011) 4878–; doi:10.1039/c0ce00897d

data_7206147
_publ_section_title
;
 Three novel supramolecular hybrid compounds based on keggin
 polytungstates
;
_journal_issue                   15
_journal_name_full               CrystEngComm
_journal_page_first              4878
_journal_paper_doi               10.1039/c0ce00897d
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C90 H72 Cu4.5 N18 O40 P W12'
_chemical_formula_weight         4568.76
_chemical_name_systematic
;
?
;
_space_group_IT_number           167
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   22.0053(5)
_cell_length_b                   22.0053(5)
_cell_length_c                   76.102(4)
_cell_measurement_temperature    296(2)
_cell_volume                     31914(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0634
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       92
_diffrn_reflns_limit_l_min       -93
_diffrn_reflns_number            57331
_diffrn_reflns_theta_full        26.06
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    13.899
_exptl_absorpt_correction_T_max  0.0849
_exptl_absorpt_correction_T_min  0.0605
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    2.853
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             25098
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.35
_refine_diff_density_max         3.455
_refine_diff_density_min         -3.564
_refine_diff_density_rms         0.580
_refine_ls_extinction_coef       0.0000256(16)
_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   1.187
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         7040
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0567P)^2^+2170.6536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1411
_reflns_number_gt                5891
_reflns_number_total             7040
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0ce00897d.txt
_cod_data_source_block           k
_cod_original_cell_volume        31913.9(19)
_cod_original_sg_symbol_H-M      R-3c
_cod_original_formula_sum        'C90 H72 Cu4.50 N18 O40 P W12'
_cod_database_code               7206147