Insertion of a phospholide unit into a metalmetal bond: Synthesis and X-ray structure of [Ru3(CO)9(nu:?1:?5-PC4H2Me2)(?1-C6H5)]
Alejandro J. Arce; Ysaura De Sanctis; Maria Cristina Goite; Ruben Machado; Yomaira Otero; Teresa Gonzalez; Inorganica Chimica Acta 392 (2012) 241–245; doi:10.1016/j.ica.2012.01.033

data_1512607
_publ_section_title
;
 Insertion of a phospholide unit into a metalmetal bond: Synthesis and
 X-ray structure of [Ru3(CO)9(nu:?1:?5-PC4H2Me2)(?1-C6H5)]
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              241
_journal_page_last               245
_journal_paper_doi               10.1016/j.ica.2012.01.033
_journal_volume                  392
_journal_year                    2012
_chemical_compound_source        Synthesis
_chemical_formula_moiety         'C21 H14 O9 Os3 P'
_chemical_formula_sum            'C21 H14 O9 Os3 P'
_chemical_formula_weight         1011.89
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                91.83(2)
_cell_angle_beta                 95.121(7)
_cell_angle_gamma                102.21(2)
_cell_formula_units_Z            2
_cell_length_a                   9.871(6)
_cell_length_b                   10.035(6)
_cell_length_c                   12.684(6)
_cell_measurement_reflns_used    8873
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      55.9770
_cell_measurement_theta_min      3.2280
_cell_volume                     1221.4(12)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics
;
SHELXLTL-NT V5.1 (Bruker AXS, 1998) and DIAMOND 
(Brandenburg, 1998)
;
_computing_publication_material
; 
SHELXLTL-NT V5.1 (Bruker AXS, 1998) and PLATON (Spek, 2003).
;
_computing_structure_refinement  'SHELXLTL-NT V5.1 (Bruker AXS, 1998)'
_computing_structure_solution    'SHELXLTL-NT V5.1 (Bruker AXS, 1998)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.767
_diffrn_measurement_device       'Mercury (2x2 bin mode)'
_diffrn_measurement_device_type  'Rigaku AFC7S Mercury'
_diffrn_measurement_method       '\w '
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0493
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13431
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         1.61
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.680
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.957
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.752
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Laminar
_exptl_crystal_F_000             910
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.716
_refine_diff_density_min         -2.032
_refine_diff_density_rms         0.247
_refine_ls_extinction_coef       0.00359(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0947
_reflns_number_gt                3990
_reflns_number_total             4519
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2012-392-241-245-3.CIF
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1512607