Highly Efficient Catalysts in Directed Oxygen-Transfer Processes: Synthesis, Structures of Novel Manganese-Containing Heteropolyanions, and Applications in Regioselective Epoxidation of Dienes with Hydrogen Peroxide
Michael Bösing; Andreas Nöh; Ina Loose; Bernt Krebs; Journal of the American Chemical Society 120 (1998) 7252–7259; doi:10.1021/ja974281v

data_4116776
_publ_contact_author
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Bernt Krebs
Anorganisch-Chemisches Institut
Westfaelische Wilhelms-Universitaet Muenster
Wilhelm-Klemm-Strasse 8
48149 Muenster
Bundesrepublik Deutschland
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_publ_contact_author_email       krebs@uni-muenster.de
_publ_contact_author_fax         '0251 833 83 66'
_publ_contact_author_phone       '0251 833 31 31'
_publ_section_title
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 Highly Efficient Catalysts in Directed Oxygen-Transfer Processes:
 Synthesis, Structures of Novel Manganese-Containing Heteropolyanions, and
 Applications in Regioselective Epoxidation of Dienes with Hydrogen
 Peroxide
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7252
_journal_page_last               7259
_journal_paper_doi               10.1021/ja974281v
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'Bi2 H102 Mn2 N4 Na6 O113 W20'
_chemical_formula_weight         6309.64
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 95.08(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.850(3)
_cell_length_b                   25.100(5)
_cell_length_c                   16.020(3)
_cell_measurement_temperature    153(2)
_cell_volume                     5146.7(19)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_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  0.0521
_diffrn_reflns_av_sigmaI/netI    0.0997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8487
_diffrn_reflns_theta_max         24.01
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    26.042
_exptl_crystal_density_diffrn    4.071
_exptl_crystal_F_000             5592
_refine_diff_density_max         4.509
_refine_diff_density_min         -3.371
_refine_diff_density_rms         0.662
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.072
_refine_ls_goodness_of_fit_obs   1.083
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         8084
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_restrained_S_obs      1.083
_refine_ls_R_factor_all          0.1247
_refine_ls_R_factor_obs          0.0789
_refine_ls_shift/esd_max         0.300
_refine_ls_shift/esd_mean        0.045
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+1100.2224P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2042
_refine_ls_wR_factor_obs         0.1594
_reflns_number_observed          5632
_reflns_number_total             8090
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja974281v_1.cif
_cod_data_source_block           abs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+1100.2224P] 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^)+(0.0550P)^2^+1100.2224P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'H102 Bi2 Mn2 N4 Na6 O113 W20'
_cod_database_code               4116776