pH-controlled and sulfite anion-directed assembly of a family of cerium(III)-containing polyoxotungstates clusters.
Chen, Wei-Chao; Wang, Xin-Long; Jiao, Yan-Qing; Huang, Peng; Zhou, En-Long; Su, Zhong-Min; Shao, Kui-Zhan; Inorganic chemistry 53 (2014) 9486–9497; doi:10.1021/ic500442k

data_4340932
_publ_section_title
;
 pH-controlled and sulfite anion-directed assembly of a family of
 cerium(III)-containing polyoxotungstates clusters.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9486
_journal_page_last               9497
_journal_paper_doi               10.1021/ic500442k
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C16 H146 Ce4 N8 Na16 O191 W44'
_chemical_formula_weight         12525.13
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           122
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.987(4)
_cell_length_b                   25.987(4)
_cell_length_c                   34.162(6)
_cell_measurement_reflns_used    6046
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.9909
_cell_measurement_theta_min      2.3847
_cell_volume                     23070(6)
_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      296(2)
_diffrn_detector_area_resol_mean 0.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX area-detector diffractometer'
_diffrn_measurement_method       '\f and \w scan'
_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  0.1201
_diffrn_reflns_av_sigmaI/netI    0.0807
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            58962
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.735
_exptl_absorpt_correction_T_max  0.0789
_exptl_absorpt_correction_T_min  0.0707
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             21960
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_platon_squeeze_details
;
;
_refine_diff_density_max         1.990
_refine_diff_density_min         -1.288
_refine_diff_density_rms         0.312
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         10158
_refine_ls_number_restraints     290
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1003
_reflns_number_gt                8616
_reflns_number_total             10158
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500442k_si_003.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4340931--4340935.cif.'
_cod_original_cell_volume        23071(6)
_cod_original_sg_symbol_H-M      I-42d
_cod_database_code               4340932