Syntheses, molecular structures and pH-dependent monomer‒dimer equilibria of Dawson α2-monotitanium(iv)-substituted polyoxometalates
Yoshida, Shoko; Murakami, Hideyuki; Sakai, Yoshitaka; Nomiya, Kenji; Dalton Transactions  (2008) 4630–; doi:10.1039/b802410c

data_7004080
_publ_section_title
;
 Syntheses, molecular structures and pH-dependent monomer--dimer
 equilibria of Dawson \a2-monotitanium(iv)-substituted polyoxometalates
;
_journal_issue                   34
_journal_name_full               'Dalton Transactions'
_journal_page_first              4630
_journal_paper_doi               10.1039/b802410c
_journal_year                    2008
_chemical_formula_sum            'H36 K12 O140 P4 Ti2 W34'
_chemical_formula_weight         9216.07
_chemical_name_systematic
;
?
;
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.888(3)
_cell_length_b                   21.473(4)
_cell_length_c                   48.571(10)
_cell_measurement_temperature    90(2)
_cell_volume                     14485(5)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_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  0.0874
_diffrn_reflns_av_sigmaI/netI    0.0967
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_number            54552
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         0.84
_exptl_absorpt_coefficient_mu    27.475
_exptl_absorpt_correction_T_max  0.4928
_exptl_absorpt_correction_T_min  0.1698
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS; Sheldrick 1996'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             16016
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         5.547
_refine_diff_density_min         -3.884
_refine_diff_density_rms         0.823
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.020(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         17955
_refine_ls_number_restraints     2124
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0686P)^2^+539.3762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1529
_reflns_number_gt                15348
_reflns_number_total             17955
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b802410c.txt
_cod_data_source_block           syo17-ortho
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      C222(1)
_cod_database_code               7004080