Getting a Clue to the Hydrolytic Activation of White Phosphorus: The Generation and Stabilization of P(OH)2PHPHPH(OH) at Ruthenium Centers
Pierluigi Barbaro; Massimo Di Vaira; Maurizio Peruzzini; Stefano Seniori Costantini; Piero Stoppioni; Inorganic Chemistry 48 (2009) 1091–1096; doi:10.1021/ic801859z

data_4301320
_publ_contact_author_address
;
Dipartimento di Chimica
Universit\'a di Firenze
Via della Lastruccia 5
I-50019 Sesto Fiorentino
Firenze
Italy
;
_publ_contact_author_email       massimo.divaira@unifi.it
_publ_contact_author_name        'Prof. Massimo Di Vaira'
_publ_contact_author_phone       '+039 055 4573278'
_publ_section_title
;
Getting a Clue to the Hydrolytic Activation of White Phosphorus: The
Generation and Stabilization of P(OH)2PHPHPH(OH) at Ruthenium Centers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1091
_journal_page_last               1096
_journal_paper_doi               10.1021/ic801859z
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C64 H61 O3 P7 Ru2 +2, 2(C F6 O6 S -)'
_chemical_formula_sum            'C66 H61 F6 O9 P7 Ru2 S2'
_chemical_formula_weight         1595.20
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.64(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.493(1)
_cell_length_b                   18.021(1)
_cell_length_c                   26.931(2)
_cell_measurement_reflns_used    33910
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      72.13
_cell_measurement_theta_min      3.91
_cell_volume                     7030.9(8)
_computing_cell_refinement
'Oxford Diffraction software, CrysAlisPro 171.29.2'
_computing_data_collection
'Oxford Diffraction software, CrysAlisPro 171.29.2'
_computing_data_reduction
'Oxford Diffraction software, CrysAlisPro 171.29.2'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 8.1241
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Oxford Diffraction Excalibur PX Ultra CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'Oxford Diffraction, Enhance ULTRA assembly'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            123158
_diffrn_reflns_theta_full        72.44
_diffrn_reflns_theta_max         72.44
_diffrn_reflns_theta_min         3.91
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.133
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSPACK (Oxford Diffraction, 2006)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'small prism'
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.412
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     928
_refine_ls_number_reflns         13824
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0912P)^2^+6.9717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1586
_reflns_number_gt                9600
_reflns_number_total             13824
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic801859z_si_001.cif
_cod_data_source_block           ru4p
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4301320