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_7219258
_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_formula_moiety         'C59 H52 N3 O P3 Ru S'
_chemical_formula_sum            'C59 H52 N3 O P3 Ru S'
_chemical_formula_weight         1045.07
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-08-06
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2014-08-26 deposited with the CCDC.
2015-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                86.469(3)
_cell_angle_beta                 79.675(3)
_cell_angle_gamma                71.360(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4861(4)
_cell_length_b                   13.3046(5)
_cell_length_c                   21.9391(9)
_cell_measurement_reflns_used    7845
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.8100
_cell_measurement_theta_min      3.7580
_cell_volume                     2581.15(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4015
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -77.00  -32.00   1.0000   26.7550
omega____ theta____ kappa____ phi______ frames
    -       10.3715  179.0000  -60.0000 45

  2 omega  -77.00  -32.00   1.0000   26.7550
omega____ theta____ kappa____ phi______ frames
    -       10.3715  179.0000   60.0000 45

  3 omega   60.00   96.00   1.0000   26.7550
omega____ theta____ kappa____ phi______ frames
    -       10.3715 -179.0000   60.0000 36

  4 omega   66.00   91.00   1.0000   26.7550
omega____ theta____ kappa____ phi______ frames
    -       10.3715 -179.0000 -120.0000 25

  5 omega  -86.00   -2.00   1.0000   26.7550
omega____ theta____ kappa____ phi______ frames
    -      -11.3871  -38.0000 -150.0000 84

  6 omega  -96.00  -51.00   1.0000   26.7550
omega____ theta____ kappa____ phi______ frames
    -      -11.3871 -179.0000  -30.0000 45

  7 omega  -94.00   38.00   1.0000   26.7550
omega____ theta____ kappa____ phi______ frames
    -      -11.3871    0.0000  -90.0000 132
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0672207000
_diffrn_orient_matrix_UB_12      0.0429573000
_diffrn_orient_matrix_UB_13      -0.0007361000
_diffrn_orient_matrix_UB_21      0.0377605000
_diffrn_orient_matrix_UB_22      0.0228492000
_diffrn_orient_matrix_UB_23      -0.0251421000
_diffrn_orient_matrix_UB_31      -0.0215642000
_diffrn_orient_matrix_UB_32      -0.0282534000
_diffrn_orient_matrix_UB_33      -0.0211495000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23377
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_min         3.368
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.481
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       prism
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         9123
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0481
_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^)+(0.0573P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1164
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6453
_reflns_number_total             9123
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ra14797a2.cif
_cod_data_source_block           ruh2p4
_cod_original_cell_volume        2581.15(18)
_cod_database_code               7219258
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'Ru1 P2 N3 S1 O1 C40 H40'
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Others
 Sof(H57)=Sof(C55A)=Sof(H55A)=Sof(C56A)=Sof(H56A)=1-FVAR(1)
 Sof(H57A)=Sof(C55)=Sof(H55)=Sof(C56)=Sof(H56)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
3.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23),
  C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32),
 C33(H33), C34(H34), C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41),
  C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C49(H49), C50(H50),
 C51(H51), C52(H52), C53(H53), C57(H57A), C57(H57), C58(H58), C59(H59),
 C55A(H55A), C56A(H56A), C55(H55), C56(H56)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_shelx_res_checksum              97787
_shelx_hkl_checksum              85032
_olex2_submission_special_instructions 'No special instructions were received'