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_4305629
_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_compound_source        synthetic
_chemical_formula_sum            'C16 H32 I2 N3 P Ru'
_chemical_formula_weight         652.29
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 103.664(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6415(7)
_cell_length_b                   15.1527(11)
_cell_length_c                   15.666(2)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      13.44
_cell_measurement_theta_min      7.37
_cell_volume                     2223.9(4)
_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-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '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  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7056
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         1.90
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Siemens P4'
_diffrn_standards_decay_%        1.5
_diffrn_standards_interval_count 147
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.556
_exptl_absorpt_correction_T_max  0.9506
_exptl_absorpt_correction_T_min  0.6363
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red-black
_exptl_crystal_density_diffrn    1.948
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhomb
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.562
_refine_diff_density_min         -1.284
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.080
_refine_ls_goodness_of_fit_obs   1.128
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         5617
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_restrained_S_obs      1.128
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_obs          0.0366
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+0.8845P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0859
_refine_ls_wR_factor_obs         0.0796
_reflns_number_observed          4474
_reflns_number_total             5619
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic800611h_si_001_1.cif
_cod_data_source_block           Compound_16
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+0.8845P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+0.8845P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2223.9(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4305629