X-ray Diffraction and NMR Studies on a Series of Binap-Based Ru(II) Hydroxyphosphine π-Arene Complexes
Tilmann J. Geldbach; Frank Breher; Volker Gramlich; P. G. Anil Kumar; Paul S. Pregosin; Inorganic Chemistry 43 (2004) 1920–1928; doi:10.1021/ic0352147

data_4310735
_publ_section_title
;
 X-ray Diffraction and NMR Studies on a Series of Binap-Based Ru(II)
 Hydroxyphosphine \p-Arene Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1920
_journal_page_last               1928
_journal_paper_doi               10.1021/ic0352147
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C146 H114 B2 F48 O8 P4 Ru2'
_chemical_formula_weight         3256.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.787(6)
_cell_angle_beta                 92.473(6)
_cell_angle_gamma                102.810(6)
_cell_formula_units_Z            1
_cell_length_a                   14.154(4)
_cell_length_b                   16.131(5)
_cell_length_c                   16.602(5)
_cell_measurement_temperature    233(2)
_cell_volume                     3472.2(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0747
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30974
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    0.386
_exptl_absorpt_correction_type   empirical(SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1091
_refine_ls_number_reflns         14185
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          2.432
_refine_ls_shift/su_mean         0.041
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0764P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1368
_reflns_number_gt                9006
_reflns_number_total             14185
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0352147si20031216_102834.cif
_cod_data_source_block           am
_cod_database_code               4310735