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_7110022
_publ_section_title
;
 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         'C28 H49 N2 O P3 Ru, C7 H8'
_chemical_formula_sum            'C35 H57 N2 O P3 Ru'
_chemical_formula_weight         715.83
_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
_audit_creation_date             2013-06-03
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.0540(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4066(7)
_cell_length_b                   21.1342(15)
_cell_length_c                   17.1162(12)
_cell_measurement_reflns_used    4269
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      2.19
_cell_volume                     3749.8(5)
_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
;
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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_unetI/netI     0.0591
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12583
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.422
_diffrn_reflns_theta_min         1.927
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.574
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.687942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0643 before and 0.0582 after correction.
 The Ratio of minimum to maximum transmission is 0.93.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1063 before and 0.0631 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 84247 reflections, Rint = 0.0861
 (24631 with I > 3sig(I), Rint = 0.0485)
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.172
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.128
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         12583
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0286P)^2^+1.4614P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0786
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9968
_reflns_number_total             12583
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc46596a.txt
_cod_data_source_block           compd5
_cod_database_code               7110022
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C7(H7)
2.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C33(H33), C34(H34), C30(H30), C31(H31), C24(H24), C25(H25),
 C26(H26), C27(H27), C28(H28), C5(H5), C4(H4), C3(H3)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C35(H35A,H35B,H35C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C19(H19A,H19B,H19C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C15(H15A,
 H15B,H15C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C),
 C11(H11A,H11B,H11C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_shelx_hkl_checksum              22846
_shelx_res_checksum              45151
_shelxl_version_number           2013-2