Aerobic Oxidation of an Osmium(III) N-Hydroxyguanidine Complex To Give Nitric Oxide.
Xiang, Jing; Wang, Qian; Yiu, Shek-Man; Man, Wai-Lun; Kwong, Hoi-Ki; Lau, Tai-Chu; Inorganic chemistry 55 (2016) 5056–5061; doi:10.1021/acs.inorgchem.6b00652

data_4347816
_publ_section_title
;
 Aerobic Oxidation of an Osmium(III) N-Hydroxyguanidine Complex To Give
 Nitric Oxide.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5056
_journal_page_last               5061
_journal_paper_doi               10.1021/acs.inorgchem.6b00652
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C17 H11 N6 O3 Os, 2(C24 H20 P), 4.5(O)'
_chemical_formula_sum            'C65 H60 N6 O7.5 Os P2'
_chemical_formula_weight         1297.33
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
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_audit_creation_date
;
'Fri Sep 11 12:29:48 2009'
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_audit_creation_method
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_computing_cell_refinement
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
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CrysAlisPro, Oxford Diffraction Ltd.,
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  1 omega  -73.00  -44.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
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  2 omega  -30.00   70.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
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  3 omega    9.00   98.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       39.7986   79.0000  -48.0000 89

  4 omega  -33.00    7.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       39.7986  -37.0000   30.0000 40

  5 omega  -97.00    6.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   25.0000    0.0000 103

  6 omega  -96.00  -53.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  179.0000   90.0000 43

  7 omega -103.00  -43.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  -77.0000   27.0000 60

  8 omega  -81.00    0.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
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  9 omega -113.00  -44.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  111.0000   90.0000 69

 10 omega   73.00  102.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0296  -92.0000  -43.0000 29

 11 omega   87.00  170.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0296   50.0000  -90.0000 83

 12 omega   40.00  121.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0296  -50.0000 -180.0000 81

 13 omega   41.00  130.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0296  -90.0000 -161.0000 89

 14 omega   56.00  127.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0296  -50.0000  -60.0000 71

 15 omega   72.00  100.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0296  -90.0000  171.0000 28

 16 omega   85.00  147.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0296  -92.0000   95.0000 62

 17 omega   78.00  142.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0296  -25.0000   60.0000 64

 18 omega  121.00  172.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0296    0.0000 -120.0000 51

 19 omega   42.00   71.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0296  -90.0000  171.0000 29

 20 omega   36.00  143.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0296  -25.0000 -120.0000 107

 21 omega  141.00  170.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0296   50.0000   90.0000 29

 22 omega   87.00  129.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0296   50.0000   90.0000 42

 23 omega   37.00  107.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0296  -92.0000  -25.0000 70

 24 omega   86.00  114.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0296  -92.0000  -83.0000 28

 25 omega   53.00  124.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0296  -50.0000    0.0000 71

 26 omega   87.00  128.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0296   50.0000  150.0000 41

 27 omega   74.00  103.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0296  -92.0000  106.0000 29

 28 omega   76.00  147.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0296  -92.0000   15.0000 71

 29 omega   10.00  110.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       39.7986   77.0000 -120.0000 100

 30 omega   10.00  110.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       39.7986   77.0000  150.0000 100

 31 omega   10.00  110.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       39.7986   77.0000   60.0000 100

 32 omega -135.00  -33.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  -79.0000 -151.0000 102

 33 omega -134.00  -34.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  -77.0000  -48.0000 100

 34 omega   87.00  178.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0296   50.0000   60.0000 91

 35 omega   75.00  178.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0296   25.0000    0.0000 103
;
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_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
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_diffrn_reflns_number            34066
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_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.784
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
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_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.263
_refine_diff_density_min         -0.749
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     723
_refine_ls_number_reflns         11144
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0774P)^2^+1.4544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1125
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_cod_data_source_file            ic6b00652_si_005.cif
_cod_data_source_block           090409b_xj
_cod_original_cell_volume        3134.14(9)
_cod_original_formula_sum        'C65 H60 N6 O7.50 Os P2'
_cod_database_code               4347816
_chemical_oxdiff_formula         'Os2 P4 O15 N12 C130'
_cell_oxdiff_angle_alpha         97.1632(13)
_cell_oxdiff_angle_beta          94.7788(14)
_cell_oxdiff_angle_gamma         106.9658(15)
_cell_oxdiff_length_a            10.8363(2)
_cell_oxdiff_length_b            16.4986(2)
_cell_oxdiff_length_c            18.6208(3)
_cell_oxdiff_measurement_reflns_used 27706
_cell_oxdiff_volume              3134.14(9)
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49