Novel ruthenium(ii) complexes containing the N-phosphorylated iminophosphorane-phosphine ligand Ph2PCH2P{NP(O)(OEt)2}Ph2: a new coordination mode of its methanide anion
Cadierno, Victorio; Díez, Josefina; García-Álvarez, Joaquín; Gimeno, José; Rubio-García, Javier; Dalton Transactions  (2008) 5737–5748; doi:10.1039/b809166h

data_7004603
_publ_section_title
;
 Novel ruthenium(ii) complexes containing the N-phosphorylated
 iminophosphorane-phosphine ligand
 Ph2PCH2P{&#xE001;NP(&#xE001;O)(OEt)2}Ph2: a new coordination mode of
 its methanide anion
;
_journal_issue                   42
_journal_name_full               'Dalton Transactions'
_journal_page_first              5737
_journal_page_last               5748
_journal_paper_doi               10.1039/b809166h
_journal_year                    2008
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C44 H51 N2 O3 P3 Ru, 0.5(C6 H14), 2(F6 Sb)'
_chemical_formula_sum            'C47 H58 F12 N2 O3 P3 Ru Sb2'
_chemical_formula_weight         1364.43
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 108.646(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.1651(10)
_cell_length_b                   11.7056(4)
_cell_length_c                   21.9561(8)
_cell_measurement_temperature    100(2)
_cell_volume                     5397.6(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'PLATON (Spek, 2007)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-99 (Beurskens, 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.813
_diffrn_measured_fraction_theta_max 0.813
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_sigmaI/netI    0.0751
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20594
_diffrn_reflns_theta_full        71.24
_diffrn_reflns_theta_max         71.24
_diffrn_reflns_theta_min         4.06
_exptl_absorpt_coefficient_mu    11.682
_exptl_absorpt_correction_T_max  0.7270
_exptl_absorpt_correction_T_min  0.2540
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick,G.M.,1997-2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2708
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.253
_refine_diff_density_min         -1.062
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     654
_refine_ls_number_reflns         8523
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1231
_refine_ls_R_factor_gt           0.0840
_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^)+(0.0767P)^2^+57.7166P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1943
_refine_ls_wR_factor_ref         0.2137
_reflns_number_gt                5648
_reflns_number_total             8523
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b809166h.txt
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               7004603