Ruthenium(II) Complexes Containing Phosphine-Functionalized Thiosemicarbazone Ligand: Synthesis, Structures and Catalytic C-N Bond Formation Reactions via N-alkylation
Ramachandran, Rangasamy; Prakash, Govind; Selvamurugan, Sellappan; Viswanathamurthi, Periasamy; Malecki, Jan; Linert, Wolfgang; Gusev, Alexey N.; RSC Adv.  (2015) –; doi:10.1039/C4RA14797A

data_7219257
_publ_section_title
;
 Ruthenium(II) Complexes Containing Phosphine-Functionalized
 Thiosemicarbazone Ligand: Synthesis, Structures and Catalytic C-N Bond
 Formation Reactions via N-alkylation
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA14797A
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C44 H42 N6 P2 Ru S2'
_chemical_formula_sum            'C44 H42 N6 P2 Ru S2'
_chemical_formula_weight         881.97
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-04-17
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2014-08-26 deposited with the CCDC.
2015-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.080(2)
_cell_length_b                   22.178(4)
_cell_length_c                   16.849(3)
_cell_measurement_reflns_used    20162
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      34.4694
_cell_measurement_theta_min      3.0293
_cell_volume                     4140.3(13)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXH-1997 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 16.0328
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_orient_matrix_UB_11      -0.0436122848
_diffrn_orient_matrix_UB_12      -0.0146331145
_diffrn_orient_matrix_UB_13      -0.0240502304
_diffrn_orient_matrix_UB_21      0.0465712695
_diffrn_orient_matrix_UB_22      -0.0106159474
_diffrn_orient_matrix_UB_23      -0.0252877618
_diffrn_orient_matrix_UB_31      0.0054375508
_diffrn_orient_matrix_UB_32      -0.0263660621
_diffrn_orient_matrix_UB_33      0.0235555757
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24015
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.04
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.596
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedra
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3654
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0325P)^2^+8.1386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0795
_reflns_number_gt                3528
_reflns_number_total             3654
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra14797a2.cif
_cod_data_source_block           rudmso
_cod_original_cell_volume        4140.2(14)
_cod_database_code               7219257
_reflns_odcompleteness_completeness 94.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     34.50
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C2(H2), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C22(H22), C21(H21), C20(H20), C19(H19), C18(H18)
2.c Fitted hexagon refined as free rotating group:
 C17(C22,C21,C20,C19,C18)
2.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;