Decomposition of A-Type Sandwiches. Synthesis and Characterization of New Polyoxometalates Incorporating Multiple d-Electron-Centered Units
Michelle D. Ritorto; Travis M. Anderson; Wade A. Neiwert; Craig L. Hill; Inorganic Chemistry 43 (2004) 44–49; doi:10.1021/ic035115t

data_4310356
_publ_contact_author_address
;
Emory University
Department of Chemistry
X-ray Crystallography Laboratory
Atlanta GA 30322-2210
USA
;
_publ_contact_author_email       khardca@emory.edu
_publ_contact_author_fax         404-727-6586
_publ_contact_author_name        'Kenneth I. Hardcastle'
_publ_contact_author_phone       404-727-6140
_publ_section_title
;
 Decomposition of A-Type Sandwiches. Synthesis and Characterization of New
 Polyoxometalates Incorporating Multiple d-Electron-Centered Units
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              44
_journal_page_last               49
_journal_paper_doi               10.1021/ic035115t
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'Co6 H21 K5 Na3 O117 P3 W24'
_chemical_formula_weight         7016.53
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.787(2)
_cell_angle_beta                 85.570(2)
_cell_angle_gamma                89.225(2)
_cell_formula_units_Z            2
_cell_length_a                   13.1585(16)
_cell_length_b                   21.060(3)
_cell_length_c                   22.891(3)
_cell_measurement_reflns_used    6990
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.83
_cell_measurement_theta_min      2.30
_cell_volume                     6224.3(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1667
_diffrn_reflns_av_sigmaI/netI    0.1520
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            47056
_diffrn_reflns_theta_full        21.72
_diffrn_reflns_theta_max         21.72
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    23.171
_exptl_absorpt_correction_T_max  0.5432
_exptl_absorpt_correction_T_min  0.0758
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    3.744
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             6136
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         9.412
_refine_diff_density_min         -3.440
_refine_diff_density_rms         1.212
_refine_ls_extinction_coef       0.00219(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     846
_refine_ls_number_reflns         14717
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.1698
_refine_ls_R_factor_gt           0.1275
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1500P)^2^+200.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2842
_refine_ls_wR_factor_ref         0.3082
_reflns_number_gt                10371
_reflns_number_total             14717
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035115tsi20030922_022240_2.cif
_cod_data_source_block           1Co
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_cell_volume        6224.2(13)
_cod_original_formula_sum        'H21 Co6 K5 Na3 O117 P3 W24'
_cod_database_code               4310356