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_4310731
_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            'C67 H43 B Cl2 F24 O3 P2 Ru'
_chemical_formula_weight         1596.73
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.614(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8389(14)
_cell_length_b                   18.934(2)
_cell_length_c                   27.128(3)
_cell_measurement_temperature    200(2)
_cell_volume                     6594.2(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX with CCD Area detector'
_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  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            67271
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.482
_exptl_absorpt_correction_type   empirical(SADABS)
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3192
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.986
_refine_diff_density_min         -1.627
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.367
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1032
_refine_ls_number_reflns         16355
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.369
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.1165
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+30.7852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2530
_refine_ls_wR_factor_ref         0.2559
_reflns_number_gt                15137
_reflns_number_total             16355
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0352147si20031216_102708.cif
_cod_data_source_block           at
_cod_original_cell_volume        6594.3(12)
_cod_database_code               4310731