Isolation of extendable transition metal incorporated polyoxometalate intermediates with structural control
Mitchell, Scott G.; Ritchie, Chris; Long, De-Liang; Cronin, Leroy; Dalton Transactions  (2008) 1415–1417; doi:10.1039/b715885h

data_7003385
_publ_section_title
;
 Isolation of extendable transition metal incorporated polyoxometalate
 intermediates with structural control
;
_journal_issue                   11
_journal_name_full               'Dalton Transactions'
_journal_page_first              1415
_journal_page_last               1417
_journal_paper_doi               10.1039/b715885h
_journal_year                    2008
_chemical_formula_sum            'Co3 H54 K2 Na12 O92 Si2 W17'
_chemical_formula_weight         5224.53
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   12.0890(12)
_cell_length_b                   21.174(2)
_cell_length_c                   33.888(4)
_cell_measurement_reflns_used    26065
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.0
_cell_measurement_theta_min      2.5
_cell_volume                     8674.4(16)
_computing_cell_refinement       Apex2
_computing_data_collection       Apex2
_computing_data_reduction        Apex2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker ApexII'
_diffrn_measurement_method       '\w & \p 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  0.0864
_diffrn_reflns_av_sigmaI/netI    0.0972
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            30303
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.20
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    23.303
_exptl_absorpt_correction_T_max  0.2282
_exptl_absorpt_correction_T_min  0.0843
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Pink
_exptl_crystal_density_diffrn    4.001
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             9279
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.69
_refine_diff_density_min         -4.71
_refine_diff_density_rms         0.53
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.44(3)
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     777
_refine_ls_number_reflns         12465
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0684
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0979P)^2^+434.0846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1618
_refine_ls_wR_factor_ref         0.1819
_reflns_number_gt                9518
_reflns_number_total             12465
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b715885h.txt
_cod_data_source_block           sm0211b
_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 

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_original_cell_volume        8674.2(17)
_cod_original_sg_symbol_H-M      P212121
_cod_original_formula_sum        'H54 Co3 K2 Na12 O92 Si2 W17'
_cod_database_code               7003385