Chiral Induction at Octahedral Ru(II) via the Disassembly of Diruthenium(II,III) Tetracarboxylates Using a Variety of Chiral Diphosphine Ligands
Brandon R. Groves; D. Ian Arbuckle; Ernest Essoun; Travis L. Lundrigan; Ruiyao Wang; Manuel A.S. Aquino; Inorganic Chemistry 52 (2013) 11563–11572; doi:10.1021/ic401908t

data_4336348
_publ_contact_author_email       maquino@stfx.ca
_publ_contact_author_fax         902-867-2414
_publ_contact_author_name        'Manuel A.S. Aquino'
_publ_contact_author_phone       902-867-5336
_publ_section_title
;
 Chiral Induction at Octahedral Ru(II) via the Disassembly of
 Diruthenium(II,III) Tetracarboxylates Using a Variety of Chiral
 Diphosphine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11563
_journal_page_last               11572
_journal_paper_doi               10.1021/ic401908t
_journal_volume                  52
_journal_year                    2013
_chemical_absolute_configuration rmad
_chemical_formula_sum            'C64.88 H68.5 F6 O3.88 P5 Ru'
_chemical_formula_weight         1280.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 97.339(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0349(1)
_cell_length_b                   23.1591(3)
_cell_length_c                   21.5330(3)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.99
_cell_measurement_theta_min      2.39
_cell_volume                     5952.46(12)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_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      180(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            63929
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    0.465
_exptl_absorpt_correction_T_max  0.9638
_exptl_absorpt_correction_T_min  0.9336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       block
_exptl_crystal_F_000             2647
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
Difference electron density maps revealed the presence of disordered PF6- and 
lattice methanol molecules, which were ultimately modeled through the
use of the SQUEEZE subroutine of the PLATON software suite. PLATON 
Reference: P. v.d. Sluis & A.L. Spek. Acta Cryst. (1990), A46, 194. 
Two smaller voids and One large void per lattice were found. Each smaller void 
comprises a total volume of 249 A3 and contributes a total of 97 or 98 
electrons, and the large void has a doubled volume but more than doubled 
electrons. 
Each smaller void was thus assigned to one disordered PF6- and 1.5 MeOH, which 
contributes 70 + 27 = 97 electrons, and ocuppies about 200 A3 in space. 
The large void was assigned to two PF6- and 4.5 MeOH molrcules, which 
contributes 70 x 2 + 4.5 x 18 = 221 electrons and occupies about 460 A3 in 
space.
The larger volume of the void may be a result of the disorder. The
contributions have been included in all derived crystal quantities.
;
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.012(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1263
_refine_ls_number_reflns         23023
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0697
_reflns_number_gt                19353
_reflns_number_total             23023
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401908t_si_004.cif
_cod_data_source_block           ma45a
_cod_original_formula_sum        'C64.88 H68.50 F6 O3.88 P5 Ru'
_cod_database_code               4336348