A 4-coordinate Ru(II) imido: unusual geometry, synthesis, and reactivity
Amrendra K. Singh; Benjamin G. Levine; Richard J. Staples; Aaron L. Odom; Chem.Commun. 49 (2013) 10799–; doi:10.1039/c3cc46596a

data_7110019
_publ_section_title
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 A 4-coordinate Ru(II) imido: unusual geometry, synthesis, and reactivity
;
_journal_name_full               Chem.Commun.
_journal_page_first              10799
_journal_paper_doi               10.1039/c3cc46596a
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C21 H44 N P3 Ru'
_chemical_formula_sum            'C21 H44 N P3 Ru'
_chemical_formula_weight         504.55
_chemical_name_systematic
;
 ? 
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_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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             2013-02-25
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 109.7670(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9737(11)
_cell_length_b                   11.6625(9)
_cell_length_c                   17.3011(13)
_cell_measurement_reflns_used    8272
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.60
_cell_measurement_theta_min      2.33
_cell_volume                     2653.4(4)
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20134
_diffrn_reflns_theta_full        24.62
_diffrn_reflns_theta_max         24.62
_diffrn_reflns_theta_min         2.15
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.778
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0630 before and 0.0543 after correction.
The Ratio of minimum to maximum transmission is 0.8912.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Chunk
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.126
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+0.8249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0751
_reflns_number_gt                3569
_reflns_number_total             4475
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc46596a.txt
_cod_data_source_block           aks02252013_0m_compd1
_cod_database_code               7110019
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H10 of C10, H5 of C5, H4 of C4, H3 of C3, H7 of C7
 At 1.5 times of:
  {H13A,H13B,H13C} of C13, {H11A,H11B,H11C} of C11, {H12A,H12B,H12C} of C12,
  {H9A,H9B,H9C} of C9, {H8A,H8B,H8C} of C8, {H21A,H21B,H21C} of C21, {H20A,H20B,
  H20C} of C20, {H19A,H19B,H19C} of C19, {H18A,H18B,H18C} of C18, {H17A,H17B,
  H17C} of C17, {H16A,H16B,H16C} of C16, {H15A,H15B,H15C} of C15, {H14A,H14B,
  H14C} of C14
2.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,
 H20B,H20C), C21(H21A,H21B,H21C)
;