Rational Synthesis of Heteroleptic Tris(chelate) Ruthenium Complexes [RuII(2-Ph-2′-Py)(L∧L)(L′∧L′)]PF6by Selective Substitution of the Ligand Trans to the Ruthenated Phenyl Ring
Boff, Bastien; Ali, Moussa; Alexandrova, Larissa; Espinosa-Jalapa, Noel Ángel; Saavedra-Díaz, Rafael Omar; Le Lagadec, Ronan; Pfeffer, Michel; Organometallics 32 (2013) 5092–; doi:10.1021/om400611t

data_4081340
_publ_section_title
;
 Rational Synthesis of Heteroleptic Tris(chelate) Ruthenium Complexes
 [RuII(2-Ph-2&#x2032;-Py)(L&#x2227;L)(L&#x2032;&#x2227;L&#x2032;)]PF6by
 Selective Substitution of the Ligand Trans to the Ruthenated Phenyl Ring
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              5092
_journal_paper_doi               10.1021/om400611t
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         '4(C37 H28  N5 Ru), 4(F6 P), C H2 Cl2'
_chemical_formula_sum            'C149 H114 Cl2 F24 N20 P4 Ru4'
_chemical_formula_weight         3239.66
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 96.6210(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   27.441(2)
_cell_length_b                   14.3073(11)
_cell_length_c                   18.6044(14)
_cell_measurement_reflns_used    6383
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.75
_cell_measurement_theta_min      2.52
_cell_volume                     7255.5(9)
_computing_cell_refinement       'SMART V 5.625 (Bruker, 1999)'
_computing_data_collection       'SMART V 5.625 (Bruker, 1999)'
_computing_data_reduction        'SAINT V 6.23A (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL  (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL  (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 0.83
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart APEX AXS CCD area detector'
_diffrn_measurement_method       '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  0.0757
_diffrn_reflns_av_sigmaI/netI    0.0878
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29524
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.578
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3268
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         6643
_refine_ls_number_restraints     431
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_gt           0.0568
_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^)+(0.0561P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1304
_reflns_number_gt                3850
_reflns_number_total             6643
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400611t_si_001.cif
_cod_data_source_block           7d
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        7255.5(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4081340
_solved_by                       'Simon Hernandez-Ortega'