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_4310355
_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            'H84 K Mn6 Na16 O136 P3 W24'
_chemical_formula_weight         7502.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.8980(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.4862(10)
_cell_length_b                   22.3071(12)
_cell_length_c                   35.1195(18)
_cell_measurement_reflns_used    8335
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.51
_cell_measurement_theta_min      2.17
_cell_volume                     13626.4(13)
_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 0.961
_diffrn_measured_fraction_theta_max 0.961
_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  0.1356
_diffrn_reflns_av_sigmaI/netI    0.1619
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            316030
_diffrn_reflns_theta_full        33.23
_diffrn_reflns_theta_max         33.23
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    20.934
_exptl_absorpt_correction_T_max  0.3665
_exptl_absorpt_correction_T_min  0.0437
_exptl_absorpt_correction_type   'analytical and multi-scan'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.657
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             13352
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         4.224
_refine_diff_density_min         -3.332
_refine_diff_density_rms         0.457
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1224
_refine_ls_number_reflns         50264
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1409
_refine_ls_R_factor_gt           0.0619
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0150P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1106
_reflns_number_gt                24528
_reflns_number_total             50264
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035115tsi20030922_022240_1.cif
_cod_data_source_block           1Mn
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
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_cod_database_code               4310355