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_4079969
_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_absolute_configuration ad
_chemical_formula_moiety         'C52 H71 Cl4 Co2 N2 O18 P6 Rh Ru2'
_chemical_formula_sum            'C52 H91 Cl4 Co2 N2 O18 P6 Rh Ru2'
_chemical_formula_weight         1782.80
_chemical_name_systematic
;
 ? 
;
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_symmetry_cell_setting           orthorhombic
_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             2012-01-19
_audit_creation_method
;
  Olex2 1.1-beta
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.55610(10)
_cell_length_b                   28.5300(2)
_cell_length_c                   28.6778(2)
_cell_measurement_reflns_used    21267
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      71.5112
_cell_measurement_theta_min      9.6149
_cell_volume                     14364.01(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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
;
XH, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'J. Appl. Cryst. (2007). 40, 609-613'
_diffrn_ambient_temperature      173.00(14)
_diffrn_detector_area_resol_mean 15.9578
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega   44.00  128.00   0.7000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -64.0000  -60.0000 120

  2 omega -124.00  -34.40   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  -57.0000  -60.0000 128

  3 omega   76.00  125.70   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000  -90.0000 71

  4 omega   73.00  121.30   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000 -180.0000 69

  5 omega  -61.00    8.30   0.7000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   38.0000   60.0000 99

  6 omega   44.00   81.80   0.7000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -111.0000  150.0000 54

  7 omega   41.00   90.00   0.7000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -111.0000  -60.0000 70

  8 omega   40.00   72.20   0.7000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  120.0000 46

  9 omega   37.00   71.30   0.7000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   90.0000 49

 10 omega   37.00   72.00   0.7000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -60.0000 50

 11 omega   86.00  175.60   0.7000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   38.0000   60.0000 128

 12 omega   86.00  175.60   0.7000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   38.0000  120.0000 128
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0014492000
_diffrn_orient_matrix_UB_12      -0.0446525000
_diffrn_orient_matrix_UB_13      0.0486579000
_diffrn_orient_matrix_UB_21      0.0471477000
_diffrn_orient_matrix_UB_22      0.0134704000
_diffrn_orient_matrix_UB_23      0.0366405000
_diffrn_orient_matrix_UB_31      -0.0263009000
_diffrn_orient_matrix_UB_32      0.0266367000
_diffrn_orient_matrix_UB_33      0.0631682000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0813
_diffrn_reflns_av_unetI/netI     0.0760
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            49491
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         67.50
_diffrn_reflns_theta_min         9.62
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35
_diffrn_source_power             1.75
_diffrn_source_target            Cu
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    11.857
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             7248
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.666
_refine_diff_density_min         -1.212
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1572
_refine_ls_number_reflns         24007
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0730P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1255
_reflns_number_gt                21978
_reflns_number_total             24007
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301114p_si_001.cif
_cod_data_source_block           erq42
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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)2(1)2(1)
_cod_database_code               4079969
_reflns_odcompleteness_completeness 97.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13