Tetranuclear Manganese-Oxo Aggregates Relevant to the Photosynthetic Water Oxidation Center. Crystal Structure, Spectroscopic Properties and Reactivity of Adamantane-Shaped [Mn4O6(bpea)4]4+ and the Reduced Mixed-Valence Analog [Mn4O6(bpea)4]3+
Christopher E. Dubé; David W. Wright; Samudranil Pal; Peter J. Bonitatebus; William H. Armstrong; Journal of the American Chemical Society 120 (1998) 3704–3716; doi:10.1021/ja973668v

data_4116719
_publ_section_title
;
 Tetranuclear Manganese-Oxo Aggregates Relevant to the Photosynthetic
 Water Oxidation Center. Crystal Structure, Spectroscopic Properties and
 Reactivity of Adamantane-Shaped [Mn4O6(bpea)4]4+ and the Reduced
 Mixed-Valence Analog [Mn4O6(bpea)4]3+
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3704
_journal_page_last               3716
_journal_paper_doi               10.1021/ja973668v
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C66 H66 Cl4 Mn4 N17 O22'
_chemical_formula_weight         1810.92
_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
_cell_angle_alpha                87.6260(10)
_cell_angle_beta                 84.7230(10)
_cell_angle_gamma                67.17
_cell_formula_units_Z            2
_cell_length_a                   13.2629(2)
_cell_length_b                   16.0216(2)
_cell_length_c                   20.6029(3)
_cell_measurement_temperature    293(2)
_cell_volume                     4017.82(10)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(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  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24783
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.828
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_F_000             1850
_refine_diff_density_max         2.247
_refine_diff_density_min         -2.919
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.313
_refine_ls_goodness_of_fit_obs   1.341
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1021
_refine_ls_number_reflns         17402
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.321
_refine_ls_restrained_S_obs      1.341
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_obs          0.0981
_refine_ls_shift/esd_max         15.000
_refine_ls_shift/esd_mean        0.331
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1020P)^2^+18.5786P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2667
_refine_ls_wR_factor_obs         0.2539
_reflns_number_observed          15380
_reflns_number_total             17410
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja973668v_2.cif
_cod_data_source_block           C66H66Cl4Mn4N17O22
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1020P)^2^+18.5786P] 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^)+(0.1020P)^2^+18.5786P] 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        4017.70(10)
_cod_database_code               4116719