Synthesis, molecular structure, and stability of a zirconocene derivative with α-Keggin mono-aluminum-substituted polyoxotungstate.
Kato, Chika Nozaki; Makino, Yuki; Unno, Wataru; Uno, Hidemitsu; Dalton transactions (Cambridge, England : 2003) 42 (2013) 1129–1135; doi:10.1039/c2dt32107f

data_7022232
_publ_section_title
;
 Synthesis, molecular structure, and stability of a zirconocene derivative
 with \a-Keggin mono-aluminum-substituted polyoxotungstate.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1129
_journal_page_last               1135
_journal_paper_doi               10.1039/c2dt32107f
_journal_volume                  42
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C20 H22 Al2 O80 P2 W22 Zr2, 6(C16 H36 N)'
_chemical_formula_sum            'C116 H238 Al2 N6 O80 P2 W22 Zr2'
_chemical_formula_weight         7340.20
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   14.8501(10)
_cell_length_b                   28.3308(19)
_cell_length_c                   47.428(3)
_cell_measurement_reflns_used    25570
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.89
_cell_measurement_theta_min      2.51
_cell_volume                     19954(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_source         'VariMax 50 kV 24 mA Rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1140
_diffrn_reflns_av_sigmaI/netI    0.1073
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            201646
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_exptl_absorpt_coefficient_mu    12.837
_exptl_absorpt_correction_T_max  0.5665
_exptl_absorpt_correction_T_min  0.1836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             13520.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.530
_refine_diff_density_min         -2.540
_refine_ls_abs_structure_details
;
Flack, H. D. (1983), Acta Cryst. A39, 876-881. 20715 Friedel Pairs
;
_refine_ls_abs_structure_Flack   0.081(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     2098
_refine_ls_number_reflns         44976
_refine_ls_number_restraints     3610
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0985
_refine_ls_R_factor_gt           0.0835
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w = 1/[\s^2^(Fo^2^)+(0.0447P)^2^+322.2970P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1542
_refine_ls_wR_factor_ref         0.1613
_reflns_number_gt                39058
_reflns_number_total             44982
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c2dt32107f.txt
_cod_data_source_block           1
_cod_original_cell_volume        19953(3)
_cod_database_code               7022232