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_7110020
_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         'C21 H44 Cu I N P3 Ru'
_chemical_formula_sum            'C21 H44 Cu I N P3 Ru'
_chemical_formula_weight         694.99
_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
_audit_creation_date             2013-05-30
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4473(2)
_cell_length_b                   16.2159(2)
_cell_length_c                   17.5870(2)
_cell_measurement_reflns_used    5537
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.63
_cell_measurement_theta_min      2.27
_cell_volume                     2979.46(8)
_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, 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 0.999
_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  0.0682
_diffrn_reflns_av_unetI/netI     0.0860
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16754
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.319
_diffrn_reflns_theta_min         1.708
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.426
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6696
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0726 before and 0.0659 after correction.
The Ratio of minimum to maximum transmission is 0.8986.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_F_000             1392
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details
;
 Flack x determined using 1429 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.004(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         5401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0157P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0693
_reflns_Friedel_coverage         0.758
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                4110
_reflns_number_total             5401
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc46596a.txt
_cod_data_source_block           aks03132013_0m_compd2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_space_group_crystal_system' value ' orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_database_code               7110020
_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:
 C5(H5), C4(H4), C3(H3)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C12(H12A,H12B,
 H12C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C19(H19A,H19B,
 H19C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C14(H14A,H14B,H14C), C15(H15A,
 H15B,H15C), C13(H13A,H13B,H13C)
;
_shelx_hkl_checksum              23742
_shelx_res_checksum              1059
_shelxl_version_number           2013-2