Ambiphilic Reactivity of a Ruthenaphosphaalkenyl: Synthesis ofP-Pyrazolylphosphaalkene Complexes of Ruthenium(0)
Trathen, Nicola; Greenacre, Victoria K.; Crossley, Ian R.; Roe, S. Mark; Organometallics 32 (2013) 2501–; doi:10.1021/om4001988

data_4080799
_publ_section_title
;
 Ambiphilic Reactivity of a Ruthenaphosphaalkenyl: Synthesis
 ofP-Pyrazolylphosphaalkene Complexes of Ruthenium(0)
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2501
_journal_paper_doi               10.1021/om4001988
_journal_volume                  32
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C44 H43 N2 O1 P3 Ru1 Si1'
_chemical_formula_sum            'C45 H45 Cl2 N2 O P3 Ru Si'
_chemical_formula_weight         922.8
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2012-10-24T13:43:27-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                84.0300(10)
_cell_angle_beta                 84.8730(10)
_cell_angle_gamma                89.7580(10)
_cell_formula_units_Z            4
_cell_length_a                   10.8579(3)
_cell_length_b                   19.3948(6)
_cell_length_c                   20.9791(6)
_cell_measurement_reflns_used    21741
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     4376.3(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.769295E-1
_diffrn_orient_matrix_UB_12      -0.278793E-1
_diffrn_orient_matrix_UB_13      0.47649E-2
_diffrn_orient_matrix_UB_21      -0.187096E-1
_diffrn_orient_matrix_UB_22      -0.53348E-2
_diffrn_orient_matrix_UB_23      0.478412E-1
_diffrn_orient_matrix_UB_31      -0.476428E-1
_diffrn_orient_matrix_UB_32      -0.433632E-1
_diffrn_orient_matrix_UB_33      -0.29509E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            58076
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         3.41
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  0.9606
_exptl_absorpt_correction_T_min  0.8536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.788
_refine_diff_density_min         -1.602
_refine_diff_density_rms         0.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.14
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     988
_refine_ls_number_reflns         17656
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.14
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0682
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+26.5951P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1538
_refine_ls_wR_factor_ref         0.1603
_reflns_number_gt                14631
_reflns_number_total             17656
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4001988_si_001.cif
_cod_data_source_block           nt14012
_cod_database_code               4080799