Novel phospholyl(diphenylphosphino)methane-ruthenium complexes: unexpected non-assisted cis to trans isomerization of [RuCl2(κ(2)-P-P')2].
Nguyen, Duc Hanh; Daran, Jean-Claude; Mallet-Ladeira, Sonia; Davin, Thomas; Maron, Laurent; Urrutigoïty, Martine; Kalck, Philippe; Gouygou, Maryse; Dalton transactions (Cambridge, England : 2003) 42 (2013) 75–81; doi:10.1039/c2dt32032k

data_7020814
_publ_section_title
;
 Novel phospholyl(diphenylphosphino)methane-ruthenium complexes:
 unexpected non-assisted cis to trans isomerization of
 [RuCl2(\k(2)-P-P')2].
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              75
_journal_page_last               81
_journal_paper_doi               10.1039/c2dt32032k
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C50 H40 Cl2 P4 Ru, C H2 Cl2'
_chemical_formula_sum            'C51 H42 Cl4 P4 Ru'
_chemical_formula_weight         1021.60
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      88
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2012-08-29 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   25.8002(14)
_cell_length_b                   25.8002(14)
_cell_length_c                   35.4669(18)
_cell_measurement_reflns_used    7336
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      19.61
_cell_measurement_theta_min      2.47
_cell_measurement_wavelength     0.71073
_cell_volume                     23609(2)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_computing_molecular_graphics
'ORTEPIII (Burnett & Johnson, 1996); Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       \w-\f
_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  0.1413
_diffrn_reflns_av_sigmaI/netI    0.0905
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            155458
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         0.98
_exptl_absorpt_coefficient_mu    0.583
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.15
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             8320
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
Some residual electron density were difficult to modelize and therefore, the
SQUEEZE function of PLATON (Spek, 2003) was used to eliminate the contribution
of the electron density in the solvent region from the intensity data, and the
solvent-free model was employed for the final refinement.
There is one large cavity of 6402 \%A^3^ per unitl cell. PLATON estimated that
this cavity contains 1549 electrons which may correspond to a mixture of
disordered solvent molecules. Owing to the synthetic procedure, one could guess
that the void is filled in by a mixture CH~2~Cl~2~ and MeOH. However we can?t
evaluate correctly the number and the ratio of these solvent molecules.
;
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         10818
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0780P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1492
_reflns_number_gt                6742
_reflns_number_total             10818
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2dt32032k.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7020814