Unexpected formation of [Ru(η5-C5H5)(PH{CH2N(CH2CH2)2O}2)(PPh3)2]BF4 - the first „piano-stool” ruthenium complex bearing secondary aminomethylphosphane ligand
Płotek, Michał; Starosta, Radosław; Komarnicka, Urszula K.; Skórska-Stania, Agnieszka; Stochel, Grazyna; Kyzioł, Agnieszka; Jezowska-Bojczuk, Malgorzata; RSC Adv.  (2014) –; doi:10.1039/C4RA13037E

data_7219001
_publ_section_title
;
 Unexpected formation of [Ru(\h5-C5H5)(PH{CH2N(CH2CH2)2O}2)(PPh3)2]BF4 -
 the first &#x201E;piano-stool&#x201D; ruthenium complex bearing secondary
 aminomethylphosphane ligand
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA13037E
_journal_year                    2014
_chemical_formula_moiety         'C51 H56  N2 O2 P3 Ru1, B1 F4'
_chemical_formula_sum            'C51 H56 B F4 N2 O2 P3 Ru'
_chemical_formula_weight         1009.77
_chemical_name_systematic
'(\h^5^-cyclopentadienyl)-bis[4-(tetrahydro-1,4-oxazino)methyl]phosphine- bis(triphenylphosphine)-ruthenium(II) tetrafluoroborate'
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      88
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-09-26T12:12:22-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2014-10-22 deposited with the CCDC.
2014-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   28.1859(1)
_cell_length_b                   28.1859(1)
_cell_length_c                   23.7177(2)
_cell_measurement_temperature    119.8(5)
_cell_volume                     18842.41(18)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      119.8(5)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            132166
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.859
_exptl_absorpt_coefficient_mu    0.493
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.9146
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8352
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.008
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         10782
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.06
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+39.1539P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.067
_refine_ls_wR_factor_ref         0.0726
_reflns_number_gt                9340
_reflns_number_total             10782
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ra13037e2.cif
_cod_data_source_block           pd109
_cod_original_cell_volume        18842.4(2)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_original_formula_sum        'C51 H56 B1 F4 N2 O2 P3 Ru1'
_cod_database_code               7219001