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_4347814
_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_absolute_configuration ad
_chemical_formula_moiety         'C24 H20 P, C16 H8 N5 O3 Os'
_chemical_formula_sum            'C40 H28 N5 O3 Os P'
_chemical_formula_weight         847.84
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-04-16
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3211(3)
_cell_length_b                   14.5428(3)
_cell_length_c                   21.0676(4)
_cell_measurement_reflns_used    11956
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.4723
_cell_measurement_theta_min      3.0362
_cell_volume                     3468.58(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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      173(2)
_diffrn_detector_area_resol_mean 16.1270
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega   -2.00   39.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -19.0000   90.0000 41

  2 omega  -65.00  -18.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -19.0000   90.0000 47

  3 omega   74.00  126.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000  -30.0000 52

  4 omega   74.00  117.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000 -150.0000 43

  5 omega  -62.00    1.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   37.0000   90.0000 63

  6 omega  -63.00  -18.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   37.0000 -150.0000 45

  7 omega   42.00   68.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   90.0000 26

  8 omega   64.00   90.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -111.0000    0.0000 26

  9 omega   39.00   72.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -180.0000 33

 10 omega   44.00   70.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000 -180.0000 26

 11 omega   44.00   77.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  150.0000 33

 12 omega   38.00   63.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  -60.0000 25

 13 omega   38.00   63.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000   90.0000 25

 14 omega   39.00   65.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000   30.0000 26

 15 omega   37.00   68.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  120.0000 31

 16 omega   89.00  175.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   50.0000  120.0000 86

 17 omega   32.00   77.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000 -180.0000 45

 18 omega  -29.00   70.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   75.0000 -112.0000 99

 19 omega -125.00  -33.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  -51.0000  -46.0000 92

 20 omega   33.00  125.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000   51.0000   99.0000 92

 21 omega   38.00   90.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -111.0000  150.0000 52

 22 omega   38.00  178.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   12.0000  -90.0000 140

 23 omega   40.00   83.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000 -120.0000 43

 24 omega   76.00  162.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   25.0000   30.0000 86
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0757153000
_diffrn_orient_matrix_UB_12      0.0874687000
_diffrn_orient_matrix_UB_13      0.0065001000
_diffrn_orient_matrix_UB_21      0.0348948000
_diffrn_orient_matrix_UB_22      -0.0071831000
_diffrn_orient_matrix_UB_23      -0.0706156000
_diffrn_orient_matrix_UB_31      -0.1073997000
_diffrn_orient_matrix_UB_32      0.0592320000
_diffrn_orient_matrix_UB_33      -0.0182556000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17466
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         3.69
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    7.758
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.172
_refine_diff_density_min         -1.255
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.022(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.282
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         6065
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.272
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0065P)^2^+12.3617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0826
_reflns_number_gt                6064
_reflns_number_total             6065
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00652_si_004.cif
_cod_data_source_block           010814a_xj
_cod_database_code               4347814
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13