Synthesis and Characterization of the Trihalophosphine Compounds of Ruthenium [RuX2(η6-cymene)(PY3)] (X = Cl, Br, Y = F, Cl, Br) and the Related PF2(NMe2) and P(NMe2)3 Compounds; Multinuclear NMR Spectroscopy and the X-ray Single Crystal Structures of [RuBr2(η6-cymene)(PF3)], [RuBr2(η6-cymene)(PF2{NMe2})], and [RuI2(η6-cymene)(P{NMe2}3)]
Ahmed M. A. Boshaala; Stephen J. Simpson; Jochen Autschbach; Shaohui Zheng; Inorganic Chemistry 47 (2008) 9279–9292; doi:10.1021/ic800611h

data_4305631
_publ_contact_author_address
;School of Biosciences,
216B Geoffrey Pope Building,
University of Exeter,
Stocker Road,
Exeter.  EX4 4QD
United Kingdom
;
_publ_contact_author_email       S.J.Simpson@exeter.ac.uk
_publ_contact_author_fax         '44 (0)1392 263434'
_publ_contact_author_name        'Dr. S.J. Simpson'
_publ_contact_author_phone       '44 (0)1392 263427'
_publ_section_title
;
Synthesis and Characterization of the Trihalophosphine Compounds of
Ruthenium [RuX2(\h6-cymene)(PY3)] (X = Cl, Br, Y = F, Cl, Br) and the
Related PF2(NMe2) and P(NMe2)3 Compounds; Multinuclear NMR Spectroscopy and
the X-ray Single Crystal Structures of [RuBr2(\h6-cymene)(PF3)],
[RuBr2(\h6-cymene)(PF2{NMe2})], and [RuI2(\h6-cymene)(P{NMe2}3)]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9279
_journal_page_last               9292
_journal_paper_doi               10.1021/ic800611h
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C12 H20 Br2 F2 N P Ru'
_chemical_formula_weight         508.15
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.033(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5131(5)
_cell_length_b                   11.3369(12)
_cell_length_c                   15.6280(12)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      13.51
_cell_measurement_theta_min      4.6
_cell_volume                     1642.0(2)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4856
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.24
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 147
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.925
_exptl_absorpt_correction_T_max  0.8508
_exptl_absorpt_correction_T_min  0.6058
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    2.055
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhomb
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       0.0049(3)
_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   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3752
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+2.1245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0756
_reflns_number_gt                3179
_reflns_number_total             3752
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800611h_si_001_3.cif
_cod_data_source_block           Compound_8
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4305631