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_7003386
_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            'Cl2 Co9 H109 K15 Na2 O148.6 Si3 W24'
_chemical_formula_weight         8217.89
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.139(2)
_cell_angle_beta                 85.279(2)
_cell_angle_gamma                82.646(2)
_cell_formula_units_Z            2
_cell_length_a                   13.4409(4)
_cell_length_b                   18.2739(5)
_cell_length_c                   28.8546(7)
_cell_measurement_reflns_used    18008
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.5761
_cell_measurement_theta_min      3.0378
_cell_volume                     6993.5(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9832
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Oxford Diffraction Gemini CCD'
_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  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0837
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            44919
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.05
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    21.324
_exptl_absorpt_correction_T_max  0.2243
_exptl_absorpt_correction_T_min  0.1067
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   ABSPACK
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.903
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7400
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.830
_refine_diff_density_min         -2.48
_refine_diff_density_rms         0.33
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1451
_refine_ls_number_reflns         25394
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0781
_reflns_number_gt                17600
_reflns_number_total             25394
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b715885h.txt
_cod_data_source_block           sm02-48
_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_original_formula_sum        'H109 Cl2 Co9 K15 Na2 O148.60 Si3 W24'
_cod_database_code               7003386