Synthesis and structural characterization of ruthenium(II) hydrido carbonyl triphenylphosphine α-diimine complexes with derivatives of 2,2'-bipyridine.
Wysocki, Waldemar; Karczmarzyk, Zbigniew; Kamecka, Anna; Acta crystallographica. Section C, Structural chemistry 81 (2025) –; doi:10.1107/S2053229625004619

data_2312870
_publ_section_title
;
 Synthesis and structural characterization of ruthenium(II) hydrido
 carbonyl triphenylphosphine &#x3b1;-diimine complexes with derivatives of
 2,2'-bipyridine.
;
_journal_coeditor_code           DG3074
_journal_issue                   7
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi               10.1107/S2053229625004619
_journal_volume                  81
_journal_year                    2025
_chemical_formula_iupac          '[Ru (H) (C18 H24 N2) (C18 H15 P)2 (C O)] P F6'
_chemical_formula_moiety         'C55 H55 N2 O P2 Ru +, F6 P -'
_chemical_formula_sum            'C55 H55 F6 N2 O P3 Ru'
_chemical_formula_weight         1067.99
_chemical_name_systematic
'Carbonyl(4,4'-di-<i>tert</i>-butyl-2,2'-bypyridine)hydridobis(triphenylphosphane)ruthenium(II) hexaflurophosphate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2yc'
_space_group_name_H-M_alt        'I 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 109.849(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.960(2)
_cell_length_b                   11.7394(5)
_cell_length_c                   31.263(2)
_cell_measurement_reflns_used    7682
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.0310
_cell_measurement_theta_min      1.8050
_cell_volume                     10342.3(12)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
ORTEP3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015) and WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS2013 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.833
_diffrn_measurement_device_type  'KM-4 CCD four-circle diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0999
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22635
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.296
_diffrn_reflns_theta_min         1.868
_exptl_absorpt_coefficient_mu    0.458
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86297
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2022)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       block
_exptl_crystal_F_000             4400
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.624
_refine_diff_density_min         -1.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         11777
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1362
_refine_ls_R_factor_gt           0.0835
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0823P)^2^+75.7001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1976
_refine_ls_wR_factor_ref         0.2338
_reflns_number_gt                7510
_reflns_number_total             11777
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            dg3074sup1.cif
_cod_data_source_block           Rudtbbpy
_cod_original_cell_volume        10342.5(13)
_cod_original_sg_symbol_H-M      'I 2/c'
_cod_database_code               2312870
_shelx_hkl_checksum              80522
_shelx_res_checksum              2668
_cod_database_fobs_code 2312870