New Routes for Multiple Derivatization of Polyoxometalates. Bis(acetato)dirhodium-11-tungstophosphate, [(PO4)W11O35{Rh2(OAc)2}]5-
Xinyi Wei; Michael H. Dickman; Michael T. Pope; Inorganic Chemistry 36 (1997) 130–131; doi:10.1021/ic960991a

data_4323292
_publ_section_title
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 New Routes for Multiple Derivatization of Polyoxometalates.
 Bis(acetato)dirhodium-11-tungstophosphate, [(PO4)W11O35{Rh2(OAc)2}]5-
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              130
_journal_page_last               131
_journal_paper_doi               10.1021/ic960991a
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C13 N15 O49 P Rh2 S2 W11'
_chemical_formula_weight         3473.54
_chemical_name_systematic
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 ? 
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_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 110.833(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.451(3)
_cell_length_b                   11.8408(14)
_cell_length_c                   25.698(3)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.60
_cell_measurement_theta_min      4.93
_cell_volume                     6384.9(14)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4/RA'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0502
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            10598
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        29.15
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    20.429
_exptl_absorpt_correction_T_max  0.1834
_exptl_absorpt_correction_T_min  0.0952
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    3.614
_exptl_crystal_description       block
_exptl_crystal_F_000             6104
_exptl_crystal_size_max          .06
_exptl_crystal_size_mid          .08
_exptl_crystal_size_min          .40
_refine_diff_density_max         3.604
_refine_diff_density_min         -3.094
_refine_diff_density_rms         0.444
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.017(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.103
_refine_ls_goodness_of_fit_obs   1.121
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         9728
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.102
_refine_ls_restrained_S_obs      1.121
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_obs          0.0468
_refine_ls_shift/esd_max         -0.085
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+327.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1146
_refine_ls_wR_factor_obs         0.1119
_reflns_number_observed          8999
_reflns_number_total             9728
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960991a.cif
_cod_data_source_block           wei
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+327.0000P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+327.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6384.8(13)
_cod_database_code               4323292