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_4072519
_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         'C55 H55 Cl P3 Ru, F6 P, 2(C H2 Cl2)'
_chemical_formula_sum            'C57 H59 Cl5 F6 P4 Ru'
_chemical_formula_weight         1260.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.06(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.067(3)
_cell_length_b                   16.140(3)
_cell_length_c                   21.951(4)
_cell_measurement_reflns_used    239
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.281
_cell_measurement_theta_min      3.240
_cell_volume                     5604.8(19)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs, 1990-2000)'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker APEX II 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  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            43673
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    0.690
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.870
_refine_diff_density_min         -1.065
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     747
_refine_ls_number_reflns         9474
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0624
_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^)+(0.0538P)^2^+34.6125P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1612
_reflns_number_gt                7678
_reflns_number_total             9474
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060752nsi20060821_082702.cif
_cod_data_source_block           PPh3dppp_2dPF6
_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_cell_volume        5604.7(19)
_cod_original_sg_symbol_H-M      'P2(1)/c  '
_cod_database_code               4072519