Deprotonation-Induced Structural Changes in SNS-Pincer Ruthenium Complexes with Secondary Thioamide Groups
Komiyama, Yoko; Kuwabara, Junpei; Kanbara, Takaki; Organometallics 33 (2014) 885–; doi:10.1021/om400969p

data_4082391
_publ_section_title
;
 Deprotonation-Induced Structural Changes in SNS-Pincer Ruthenium
 Complexes with Secondary Thioamide Groups
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              885
_journal_paper_doi               10.1021/om400969p
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C56 H43 N3 O P2 Ru S2'
_chemical_formula_sum            'C56 H43 N3 O P2 Ru S2'
_chemical_formula_weight         1001.11
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_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
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   15.6888(15)
_cell_length_b                   17.0438(16)
_cell_length_c                   17.3043(17)
_cell_measurement_reflns_used    5340
_cell_measurement_temperature    90
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.37
_cell_volume                     4627.1(8)
_computing_cell_refinement       Unknown
_computing_data_collection       Unknown
_computing_data_reduction        Unknown
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26469
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.543
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6072
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
SADABS V2008/1 (Bruker AXS) 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       nONE
_exptl_crystal_F_000             2056.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.900
_refine_diff_density_min         -0.440
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  4518 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     586
_refine_ls_number_reflns         10344
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0337P)^2^+0.2395P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0848
_reflns_number_gt                8539
_reflns_number_total             10344
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om400969p_si_001.cif
_cod_data_source_block           kmy124
_cod_database_code               4082391