Selective Insertion of Oxygen and Selenium into an Electron-Precise Paramagnetic Selenium-Manganese Carbonyl Cluster [Se6Mn6(CO)18]4-
Minghuey Shieh; Chia-Hua Ho; Wen-Shyan Sheu; Horng-Wen Chen; Journal of the American Chemical Society 132 (2010) 4032–4033; doi:10.1021/ja9091566

data_4102164
_publ_section_title
;
 Selective Insertion of Oxygen and Selenium into an Electron-Precise
 Paramagnetic Selenium-Manganese Carbonyl Cluster [Se6Mn6(CO)18]4-
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4032
_journal_page_last               4033
_journal_paper_doi               10.1021/ja9091566
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C25 H40 Mn3 N2 O9 Se3'
_chemical_formula_sum            'C25 H40 Mn3 N2 O9 Se3'
_chemical_formula_weight         914.29
_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                104.0210(10)
_cell_angle_beta                 97.0140(10)
_cell_angle_gamma                110.2910(10)
_cell_formula_units_Z            2
_cell_length_a                   10.2800(2)
_cell_length_b                   12.0770(2)
_cell_length_c                   15.1550(3)
_cell_measurement_reflns_used    32090
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.037
_cell_volume                     1667.67(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'HKL Denzo and Scalepack'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0639
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22014
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    4.441
_exptl_absorpt_correction_T_max  0.45
_exptl_absorpt_correction_T_min  0.2833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.821
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             906
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         3.415
_refine_diff_density_min         -1.915
_refine_diff_density_rms         0.320
_refine_ls_extinction_coef       0.0123(13)
_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   1.123
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5875
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0689
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+9.7045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1807
_refine_ls_wR_factor_ref         0.1948
_reflns_number_gt                5184
_reflns_number_total             5875
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9091566_si_002.cif
_cod_data_source_block           '[Et4N]4[1]'
_cod_original_cell_volume        1667.67(5)
_cod_database_code               4102164