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_4347817
_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 H13 N7 O3 Os, C24 H20 P, C H4 O'
_chemical_formula_sum            'C42 H37 N7 O4 Os P'
_chemical_formula_weight         924.96
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date
;
'Thu Jun 18 17:26:16 2009'
;
_audit_creation_method
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_cell_angle_alpha                99.220(2)
_cell_angle_beta                 90.675(2)
_cell_angle_gamma                101.913(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3167(2)
_cell_length_b                   12.3418(3)
_cell_length_c                   15.8830(4)
_cell_measurement_reflns_used    11127
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.7312
_cell_measurement_theta_min      3.7117
_cell_volume                     1951.10(8)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1270
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega  -87.00  -43.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.1695  125.0000   30.0000 44

  2 omega  -74.00  -47.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.1695  125.0000   60.0000 27

  3 omega  -85.00   -5.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.1695  109.0000  -84.0000 80

  4 omega  -30.00   65.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       39.1695  -77.0000  120.0000 95

  5 omega    9.00  101.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       39.1695   77.0000 -120.0000 92

  6 omega -106.00  -30.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  -25.0000  150.0000 76

  7 omega  -83.00    0.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   50.0000   90.0000 83

  8 omega -126.00  -46.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  -50.0000  150.0000 80

  9 omega   74.00  119.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4046   25.0000   90.0000 45

 10 omega  129.00  172.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4046   50.0000  -60.0000 43

 11 omega   37.00  146.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4046  -92.0000  -23.0000 109

 12 omega   78.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4046  -92.0000 -101.0000 27

 13 omega   87.00  114.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4046   50.0000  -60.0000 27

 14 omega  143.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4046   77.0000 -120.0000 35

 15 omega   37.00  138.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4046  -25.0000  120.0000 101

 16 omega   65.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4046  -92.0000  108.0000 40

 17 omega  120.00  157.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4046   77.0000  120.0000 37

 18 omega   78.00  108.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4046   77.0000  120.0000 30

 19 omega   91.00  143.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4046   50.0000    0.0000 52

 20 omega   88.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4046   50.0000   90.0000 89

 21 omega  124.00  149.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4046   77.0000 -180.0000 25

 22 omega   63.00  125.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4046  -50.0000  -60.0000 62

 23 omega   41.00  126.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4046  -90.0000 -157.0000 85

 24 omega   47.00  114.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4046  -50.0000 -180.0000 67
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0456817643
_diffrn_orient_matrix_UB_12      0.1185445481
_diffrn_orient_matrix_UB_13      -0.0221847519
_diffrn_orient_matrix_UB_21      0.0149059141
_diffrn_orient_matrix_UB_22      -0.0515755723
_diffrn_orient_matrix_UB_23      -0.0933594512
_diffrn_orient_matrix_UB_31      -0.1449212294
_diffrn_orient_matrix_UB_32      0.0033579391
_diffrn_orient_matrix_UB_33      -0.0213390832
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13101
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         3.71
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.982
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
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            red
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             922
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         6870
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0593
_reflns_number_gt                6369
_reflns_number_total             6870
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00652_si_002.cif
_cod_data_source_block           061709a
_cod_original_cell_volume        1951.11(8)
_cod_database_code               4347817
_cell_oxdiff_angle_alpha         99.220(2)
_cell_oxdiff_angle_beta          90.675(2)
_cell_oxdiff_angle_gamma         101.913(2)
_cell_oxdiff_length_a            10.3167(2)
_cell_oxdiff_length_b            12.3418(3)
_cell_oxdiff_length_c            15.8830(4)
_cell_oxdiff_measurement_reflns_used 11127
_cell_oxdiff_volume              1951.11(8)
_reflns_odcompleteness_completeness 98.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49