Heteroatom-Controlled Kinetics of Switchable Polyoxometalate Frameworks
Johannes Thiel; Chris Ritchie; Carsten Streb; De-Liang Long; Leroy Cronin; Journal of the American Chemical Society 131 (2009) 4180–4181; doi:10.1021/ja809422k

data_4104097
_publ_section_title
;
 Heteroatom-Controlled Kinetics of Switchable Polyoxometalate Frameworks
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4180
_journal_page_last               4181
_journal_paper_doi               10.1021/ja809422k
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety
'40(C4 H10 N O +), (H12 W72 Mn12 O268 Ge7 40-), 48(H2 O), 5(C6 H6 O6)'
_chemical_formula_sum            'C190 H538 Ge7 Mn12 N40 O386 W72'
_chemical_formula_weight         23964.98
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           220
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I -4bd 2c 3'
_symmetry_space_group_name_H-M   'I -4 3 d'
_atom_sites_solution_hydrogens   none
_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                   39.2899(6)
_cell_length_b                   39.2899(6)
_cell_length_c                   39.2899(6)
_cell_measurement_reflns_used    4010
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      51.3
_cell_measurement_theta_min      3.54
_cell_volume                     60651.7(16)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Gemini CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1610
_diffrn_reflns_av_sigmaI/netI    0.1119
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            20967
_diffrn_reflns_theta_full        47.46
_diffrn_reflns_theta_max         47.46
_diffrn_reflns_theta_min         3.56
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    27.541
_exptl_absorpt_correction_T_max  0.303
_exptl_absorpt_correction_T_min  0.200
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.529
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             41792
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.40
_refine_diff_density_min         -0.81
_refine_diff_density_rms         0.19
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.10(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         4614
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1766
_refine_ls_R_factor_gt           0.1200
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3157
_refine_ls_wR_factor_ref         0.3592
_reflns_number_gt                2395
_reflns_number_total             4614
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja809422k_si_001_2.cif
_cod_data_source_block           compound2red
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4104097