Reactions of a Ruthenium(VI) Nitride with Rhodium(III) and Iridium(III) Aryl Complexes. Insertion of the Ru≡N Group into the Rh‒C Bonds of Trimesitylrhodium(III)
Kwan Huang, Enrique; Cheung, Wai-Man; Sung, Herman H. Y.; Williams, Ian D.; Leung, Wa-Hung; Organometallics 32 (2013) 733–; doi:10.1021/om301114p

data_4079970
_publ_section_title
;
 Reactions of a Ruthenium(VI) Nitride with Rhodium(III) and Iridium(III)
 Aryl Complexes. Insertion of the Ru\\tb N Group into the Rh--C Bonds of
 Trimesitylrhodium(III)
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              733
_journal_paper_doi               10.1021/om301114p
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C59 H86 Cl2 Co Ir N3 O12 P3 Ru, 2(H2 O)'
_chemical_formula_sum            'C59 H90 Cl2 Co Ir N3 O14 P3 Ru'
_chemical_formula_weight         1581.35
_chemical_name_systematic
;
 ? 
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-10-11
_audit_creation_method
;
  Olex2 1.1-beta
  (compiled Sep 28 2011 20:31:00, GUI svn.r3868)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.786(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1192(5)
_cell_length_b                   20.7432(5)
_cell_length_c                   25.3514(8)
_cell_measurement_reflns_used    5856
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      71.8823
_cell_measurement_theta_min      3.4266
_cell_volume                     6777.1(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_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      173.00(14)
_diffrn_detector_area_resol_mean 15.9578
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega   39.00   69.00   1.0000   46.5909
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000   60.0000 30

  2 omega  -69.00   21.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   60.0000 90

  3 omega  -17.00   85.00   1.0000   46.5909
omega____ theta____ kappa____ phi______ frames
    -       55.0000  -99.0000   60.0000 102

  4 omega  -17.00   74.00   1.0000   46.5909
omega____ theta____ kappa____ phi______ frames
    -       55.0000  -99.0000  -90.0000 91

  5 omega   -3.00   75.00   1.0000   46.5909
omega____ theta____ kappa____ phi______ frames
    -       55.0000 -125.0000 -120.0000 78

  6 omega -134.00  -50.00   1.0000   46.5909
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  -50.0000  120.0000 84

  7 omega   39.00   72.00   1.0000   46.5909
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -60.0000 33

  8 omega   47.00  164.00   1.0000   46.5909
omega____ theta____ kappa____ phi______ frames
    -      110.0000    0.0000  150.0000 117

  9 omega   40.00   71.00   1.0000   46.5909
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000   90.0000 31

 10 omega   38.00   71.00   1.0000   46.5909
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000   30.0000 33

 11 omega   40.00   67.00   1.0000   46.5909
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000 -150.0000 27

 12 omega   40.00   82.00   1.0000   46.5909
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000    0.0000 42

 13 omega   37.00   67.00   1.0000   46.5909
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  150.0000 30

 14 omega   37.00   72.00   1.0000   46.5909
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -90.0000 35

 15 omega   45.00   74.00   1.0000   46.5909
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -111.0000 -150.0000 29

 16 omega   52.00  148.00   1.0000   46.5909
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -92.0000   90.0000 96

 17 omega   43.00   68.00   1.0000   46.5909
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000 -180.0000 25

 18 omega   45.00   83.00   1.0000   46.5909
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000 -120.0000 38

 19 omega  124.00  149.00   1.0000   46.5909
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -93.0000   12.0000 25

 20 omega   88.00  178.00   1.0000   46.5909
omega____ theta____ kappa____ phi______ frames
    -      110.0000   50.0000 -180.0000 90

 21 omega   51.00  135.00   1.0000   46.5909
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -92.0000 -120.0000 84

 22 omega   29.00  125.00   1.0000   46.5909
omega____ theta____ kappa____ phi______ frames
    -       55.0000   77.0000  -30.0000 96

 23 omega   43.00  111.00   1.0000   46.5909
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -93.0000   12.0000 68
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0381659000
_diffrn_orient_matrix_UB_12      0.0638055000
_diffrn_orient_matrix_UB_13      -0.0280194000
_diffrn_orient_matrix_UB_21      0.1130412000
_diffrn_orient_matrix_UB_22      0.0197560000
_diffrn_orient_matrix_UB_23      -0.0002346000
_diffrn_orient_matrix_UB_31      -0.0061363000
_diffrn_orient_matrix_UB_32      -0.0325035000
_diffrn_orient_matrix_UB_33      -0.0551761000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0879
_diffrn_reflns_av_unetI/netI     0.0940
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            41697
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         67.49
_diffrn_reflns_theta_min         3.55
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_source_current           40
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    9.299
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             3216
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.983
_refine_diff_density_min         -1.642
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         12140
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0251P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1081
_reflns_number_gt                8725
_reflns_number_total             12140
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301114p_si_001.cif
_cod_data_source_block           erq33cult
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4079970
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13