High versatility of 3,4-dimethyl-1-phenyl-phosphole and 3-methyl-1-phenyl-phosphole as ligands in the reaction with [Re2(CO)8(CH3CN)2] and [Ru3(CO)12]: X-ray structures of [Re2(CO)7(n1:n2:n2-PhPC4H2Me2)], [Re2(CO)7(n1:n2:n2-PhPC4H3Me)] and [Ru2(CO)4(PhPC4H3Me)2]
Yomaira Otero; Alejandro Arce; Ysaura De Sanctis; Ruben Machado; Maria C. Goite; Teresa Gonzalez; Alexander Briceno; Inorganica Chimica Acta 404 (2013) 77–81; doi:

data_1517712
_publ_section_title
;
 High versatility of 3,4-dimethyl-1-phenyl-phosphole and
 3-methyl-1-phenyl-phosphole as ligands in the reaction with
 [Re2(CO)8(CH3CN)2] and [Ru3(CO)12]: X-ray structures of
 [Re2(CO)7(n1:n2:n2-PhPC4H2Me2)], [Re2(CO)7(n1:n2:n2-PhPC4H3Me)] and
 [Ru2(CO)4(PhPC4H3Me)2]
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              77
_journal_page_last               81
_journal_volume                  404
_journal_year                    2013
_chemical_compound_source        Synthesis
_chemical_formula_moiety         'C29 H20 O4 P2 Ru2'
_chemical_formula_sum            'C29 H20 O4 P2 Ru2'
_chemical_formula_weight         696.53
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.571(9)
_cell_length_b                   15.571(9)
_cell_length_c                   12.103(8)
_cell_measurement_reflns_used    6467
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      54.2870
_cell_measurement_theta_min      3.7026
_cell_volume                     2934(3)
_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 0.909
_diffrn_measured_fraction_theta_max 0.752
_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  0.1046
_diffrn_reflns_av_sigmaI/netI    0.0645
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13840
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.71
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.169
_exptl_absorpt_correction_T_max  0.644
_exptl_absorpt_correction_T_min  0.574
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.38
_refine_diff_density_max         3.146
_refine_diff_density_min         -1.219
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         1359
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1085
_refine_ls_R_factor_gt           0.0911
_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^)+(0.1737P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2387
_refine_ls_wR_factor_ref         0.2572
_reflns_number_gt                1005
_reflns_number_total             1359
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-404-77-81-3.cif
_cod_data_source_block           shelxlsr
_cod_original_sg_symbol_Hall     -I4
_cod_original_sg_symbol_H-M      I4/m
_cod_database_code               1517712