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_7003384
_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 H58 K9 Na3 O92.7 Si2 W17'
_chemical_formula_weight         5320.95
_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                82.947(3)
_cell_angle_beta                 78.214(3)
_cell_angle_gamma                79.073(3)
_cell_formula_units_Z            2
_cell_length_a                   12.7351(6)
_cell_length_b                   18.3684(8)
_cell_length_c                   19.3171(9)
_cell_measurement_reflns_used    4386
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.5
_cell_volume                     4326.6(3)
_computing_cell_refinement       ApexII
_computing_data_collection       ApexII
_computing_data_reduction        ApexII
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0945
_diffrn_reflns_av_sigmaI/netI    0.1224
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45471
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.50
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    23.653
_exptl_absorpt_correction_T_max  0.1806
_exptl_absorpt_correction_T_min  0.1003
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    4.084
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4741
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.77
_refine_diff_density_min         -3.08
_refine_diff_density_rms         0.46
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1017
_refine_ls_number_reflns         15051
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0393P)^2^+23.0317P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1200
_reflns_number_gt                9815
_reflns_number_total             15051
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b715885h.txt
_cod_data_source_block           sm0152kcl
_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_sg_symbol_H-M      P-1
_cod_original_formula_sum        'H58 Co3 K9 Na3 O92.70 Si2 W17'
_cod_database_code               7003384