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_4080800
_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         'C47 H45 Cl2 Hg O P3 Ru Si, 1.5(C7 H8) '
_chemical_formula_sum            'C57.5 H57 Cl2 Hg O P3 Ru Si'
_chemical_formula_weight         1257.59
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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             2013-02-08T16:46:57-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 104.3576(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.3342(2)
_cell_length_b                   11.92180(10)
_cell_length_c                   43.0554(5)
_cell_measurement_reflns_used    14624
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_measurement_wavelength     0.71073
_cell_volume                     10608.77(18)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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      0.392556E-1
_diffrn_orient_matrix_UB_12      0.442742E-1
_diffrn_orient_matrix_UB_13      -0.10128E-2
_diffrn_orient_matrix_UB_21      0.143144E-1
_diffrn_orient_matrix_UB_22      0
_diffrn_orient_matrix_UB_23      0.23945E-1
_diffrn_orient_matrix_UB_31      0.243954E-1
_diffrn_orient_matrix_UB_32      -0.712435E-1
_diffrn_orient_matrix_UB_33      -0.6294E-3
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1016
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            91405
_diffrn_reflns_theta_full        27.19
_diffrn_reflns_theta_max         27.19
_diffrn_reflns_theta_min         3.42
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    3.429
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.5418
_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    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5016
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.859
_refine_diff_density_min         -0.85
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         11651
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0562P)^2^+16.6042P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1101
_reflns_number_gt                8627
_reflns_number_total             11651
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4001988_si_002.cif
_cod_data_source_block           vg58
_cod_original_cell_volume        10608.75(18)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C57.50 H57 Cl2 Hg O P3 Ru Si'
_cod_database_code               4080800