Dual Pathways in the Oxidation of an Osmium(III) Guanidine Complex. Formation of Osmium(VI) Nitrido and Osmium Nitrosyl Complex.
Xiang, Jing; Wang, Qian; Yiu, Shek-Man; Lau, Tai-Chu; Inorganic chemistry 56 (2017) 2022–2028; doi:10.1021/acs.inorgchem.6b02645

data_4345086
_publ_section_title
;
 Dual Pathways in the Oxidation of an Osmium(III) Guanidine Complex.
 Formation of Osmium(VI) Nitrido and Osmium Nitrosyl Complex.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2022
_journal_page_last               2028
_journal_paper_doi               10.1021/acs.inorgchem.6b02645
_journal_volume                  56
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C16 H8 N5 O2 Os, C24 H20 P'
_chemical_formula_sum            'C40 H28 N5 O2 Os P'
_chemical_formula_weight         831.84
_chemical_name_systematic
;
 ? 
;
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-10-30
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.59210(10)
_cell_length_b                   13.85260(10)
_cell_length_c                   21.0122(2)
_cell_measurement_reflns_used    17270
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.6332
_cell_measurement_theta_min      3.8100
_cell_volume                     3374.15(5)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_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   20.00   64.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   60.0000 44

  2 omega  -21.00   11.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   60.0000 32

  3 omega  -20.00   21.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -90.0000 41

  4 omega  -68.00  -24.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -90.0000 44

  5 omega   16.00   42.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  150.0000 26

  6 omega -123.00  -48.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  -57.0000   30.0000 75

  7 omega -112.00  -18.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  125.0000  120.0000 94

  8 omega -109.00  -27.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  -77.0000  -30.0000 82

  9 omega -120.00  -41.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  -57.0000   90.0000 79

 10 omega   -8.00   74.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  -57.0000 -150.0000 82

 11 omega -129.00 -102.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  -50.0000    0.0000 27

 12 omega -108.00  -71.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  178.0000  -60.0000 37

 13 omega   39.00   71.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -90.0000 32

 14 omega   44.00   69.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -46.0000  -83.0000 25

 15 omega   39.00   65.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  -30.0000 26

 16 omega   40.00   66.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000   90.0000 26

 17 omega   39.00   72.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -120.0000 33

 18 omega   71.00  146.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000 -140.0000 75

 19 omega  121.00  146.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000   14.0000 25

 20 omega   41.00   68.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000    0.0000 27

 21 omega   38.00   63.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   30.0000 25

 22 omega   98.00  126.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000   79.0000 28

 23 omega   41.00   67.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  150.0000 26

 24 omega   37.00   64.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   60.0000 27

 25 omega   48.00   83.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  120.0000 35

 26 omega   44.00   70.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000    0.0000 26

 27 omega   39.00  178.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -12.0000   60.0000 139

 28 omega   41.00   69.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  -60.0000 28

 29 omega   39.00   64.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -60.0000 25

 30 omega  126.00  173.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   50.0000 -120.0000 47

 31 omega   88.00  115.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   50.0000 -120.0000 27

 32 omega   41.00   73.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000 -150.0000 32

 33 omega   39.00   72.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -150.0000 33

 34 omega   79.00  106.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  -60.0000 27

 35 omega   38.00   71.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000   79.0000 33

 36 omega   41.00  111.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000   14.0000 70

 37 omega   43.00  137.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  108.0000 94
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1091817000
_diffrn_orient_matrix_UB_12      0.0065500000
_diffrn_orient_matrix_UB_13      -0.0415964000
_diffrn_orient_matrix_UB_21      0.0019480000
_diffrn_orient_matrix_UB_22      -0.1108396000
_diffrn_orient_matrix_UB_23      -0.0060321000
_diffrn_orient_matrix_UB_31      -0.0758464000
_diffrn_orient_matrix_UB_32      0.0065860000
_diffrn_orient_matrix_UB_33      -0.0600209000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23451
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         3.82
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    7.939
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48237
_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            yellow
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.022(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         6017
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0152
_refine_ls_R_factor_gt           0.0148
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+1.4101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0370
_refine_ls_wR_factor_ref         0.0371
_reflns_number_gt                5966
_reflns_number_total             6017
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b02645_si_002.cif
_cod_data_source_block           102813a_xj
_cod_depositor_comments
'Adding full bibliography for 4345086--4345087.cif.'
_cod_database_code               4345086
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13