Reaction of [Os(en)2O2]2+ with Photolyzed [Mo(CN)8]4- in Water
R. Kent Murmann; Charles L. Barnes; Inorganic Chemistry 40 (2001) 6514–6517; doi:10.1021/ic010466y

data_4320633
_publ_contact_author_address
;
  Department of Chemistry
  University of Missouri
  Columbia, MO
  65211
;
_publ_contact_author_email       murmannr@missouri.edu
_publ_contact_author_fax         573-882-2754
_publ_contact_author_name
;
R. Kent Murmann
;
_publ_contact_author_phone       573-882-2826
_publ_section_title
;
 Reaction of [Os(en)2O2]2+ with Photolyzed [Mo(CN)8]4- in Water
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6514
_journal_page_last               6517
_journal_paper_doi               10.1021/ic010466y
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         '{Co-sepulcherate)(W(CN)7(O2} 4(H2O)'
_chemical_formula_sum            'C21 H32 Co N13 O6 W'
_chemical_formula_weight         805.38
_chemical_name_systematic
;
  [Cobalt(III) sepulcherate] heptacyano-(2-peroxo
  tungsten(VI) tetra-hydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 103.397(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.2689(14)
_cell_length_b                   13.2323(13)
_cell_length_c                   15.2384(16)
_cell_measurement_reflns_used    4424
_cell_measurement_temperature    293(2)
_cell_volume                     2798.9(5)
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'ORTEP-III (Burnett & Johnson, 1996)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8496
_diffrn_reflns_theta_full        27.11
_diffrn_reflns_theta_max         27.11
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    4.762
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Data were corrected for decay and absorption using the program SADABS
  based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995).
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.911
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.342
_refine_diff_density_min         -1.187
_refine_diff_density_rms         0.174
_refine_ls_extinction_coef       0.00000(7)
_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   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3082
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.361
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+4.7449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0957
_reflns_number_gt                2668
_reflns_number_total             3082
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010466y_2.cif
_cod_data_source_block           global
_cod_database_code               4320633