Synthesis and structural characterizations of three carbonyl(α-diimine)hydrido(triphenylphosphine)ruthenium(II) complexes with derivatives of 1,10-phenanthroline.
Wysocki, Waldemar; Kamecka, Anna; Karczmarzyk, Zbigniew; Acta crystallographica. Section C, Structural chemistry 80 (2024) 319–330; doi:10.1107/S2053229624005898

data_2312529
_publ_section_title
;
 Synthesis and structural characterizations of three
 carbonyl(&#x3b1;-diimine)hydrido(triphenylphosphine)ruthenium(II)
 complexes with derivatives of 1,10-phenanthroline.
;
_journal_coeditor_code           YD3043
_journal_issue                   'Pt 7'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              319
_journal_page_last               330
_journal_paper_doi               10.1107/S2053229624005898
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '[Ru H (C14 H12 N2) (C18 H15 P)2 (C O)] P F6'
_chemical_formula_moiety         'C51 H43 N2 O P2 Ru +, F6 P -'
_chemical_formula_sum            'C51 H43 F6 N2 O P3 Ru'
_chemical_formula_weight         1007.85
_chemical_name_systematic
'Carbonylhydrido(4,7-dimethyl-1,10-phenanthroline-\k^2^<i>N</i>,<i>N</i>)bis(triphenylphosphane-\k<i>P</i>)ruthenium(II) hexafluoridophosphate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/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                 109.266(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9624(8)
_cell_length_b                   21.9572(7)
_cell_length_c                   17.1148(9)
_cell_measurement_reflns_used    6785
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.7630
_cell_measurement_theta_min      2.2900
_cell_volume                     5307.9(5)
_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
;
ORTEP-3 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      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_device_type  'KM4 CCD four-circle'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25375
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.792
_diffrn_reflns_theta_min         2.393
_exptl_absorpt_coefficient_mu    0.442
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis PRO (Rigaku OD, 2022)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_description       needle
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.702
_refine_ls_extinction_coef       0.00095(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         11913
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+3.0506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1253
_reflns_number_gt                8859
_reflns_number_total             11913
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yd3043sup1.cif
_cod_data_source_block           3_Ru47dmphen
_cod_depositor_comments
'Adding full bibliography for 2312527--2312529.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2312529
_cod_database_fobs_code          2312529
_shelx_hkl_checksum              64665
_shelx_res_checksum              40992
_shelx_fab_checksum              69592