Mechanistic Studies on the Formation of η2-Diphosphine (η6-p-cymene)ruthenium(II) Compounds
Chaplin, Adrian B.; Fellay, Céline; Laurenczy, Gábor; Dyson, Paul J.; Organometallics 26 (2007) 586–; doi:10.1021/om060752n

data_4072517
_publ_section_title
;
 Mechanistic Studies on the Formation of \h2-Diphosphine
 (\h6-p-cymene)ruthenium(II) Compounds
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              586
_journal_paper_doi               10.1021/om060752n
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C53 H51 Cl P3 Ru, F6 P, C H2 Cl2'
_chemical_formula_sum            'C54 H53 Cl3 F6 P4 Ru'
_chemical_formula_weight         1147.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 107.004(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9506(7)
_cell_length_b                   18.7248(11)
_cell_length_c                   21.1365(13)
_cell_measurement_reflns_used    7283
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      23.422
_cell_measurement_theta_min      2.066
_cell_volume                     5280.0(5)
_computing_cell_refinement       'Oxford Diffraction CrysAlis RED'
_computing_data_collection       'Oxford Diffraction CrysAlis CCD'
_computing_data_reduction        'Oxford Diffraction CrysAlis RED'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Oxford Diffraction KM4/Sapphire CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_sigmaI/netI    0.0640
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30281
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.27
_refine_diff_density_max         3.217
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         9226
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0733
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1648P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2201
_refine_ls_wR_factor_ref         0.2396
_reflns_number_gt                6468
_reflns_number_total             9226
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060752nsi20060821_082702.cif
_cod_data_source_block           PPh3dppm_2aPF6
_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.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P2(1)/n   '
_cod_database_code               4072517