Optically Active Ortho-Metalated Half-Sandwich Ruthenium Complexes: Solid-State NMR as a Convenient Tool To Analyze Mixtures of Diastereomers
Vincent Ritleng; Philippe Bertani; Michel Pfeffer; Claude Sirlin; Jérôme Hirschinger; Inorganic Chemistry 40 (2001) 5117–5122; doi:10.1021/ic010204w

data_4320292
_publ_contact_author_address
;Laboratoire de Syntheses Metallo-Induites
   UMR CNRS 7513
   Universite Louis Pasteur
   4, rue Blaise Pascal
   67070 Strasbourg Cedex
   France
;
_publ_contact_author_email       pfeffer@chimie.u-strasbg.fr
_publ_contact_author_fax         '00 33 3 90 24 15 26'
_publ_contact_author_name        ' Michel Pfeffer'
_publ_contact_author_phone       '00 33 3 90 24 15 22'
_publ_section_title
;
 Optically Active Ortho-Metalated Half-Sandwich Ruthenium Complexes:
 Solid-State NMR as a Convenient Tool To Analyze Mixtures of Diastereomers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5117
_journal_page_last               5122
_journal_paper_doi               10.1021/ic010204w
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'C24 H31 F6 N P2 Ru'
_chemical_formula_sum            'C24 H31 F6 N P2 Ru'
_chemical_formula_weight         610.53
_chemical_name_systematic        ' ?'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_date             9-10-00
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8196(2)
_cell_length_b                   13.4161(4)
_cell_length_c                   15.8619(5)
_cell_measurement_reflns_used    5784
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.4
_cell_volume                     2515.27(12)
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      173
_diffrn_measurement_details
;
     5784 reflections were collected using program Collect
   ("Collect" Data collection software, Nonius B.V., 1998)
   The conditions were as follow : crystal to detector distance =  35. mm.
   Scan angle =  2.0 deg 1 scans of   20 sec per frame.
   Data collection was divided into  2 set(s)
   with the following starting angles and number of frames :

   Set 1 Theta =    6.31 Omega =    0.00 Kappa =    0.00   84 frames
   Set 2 Theta =   -6.31 Kappa =  137.50 Phi   =    0.00   20 frames
   Friedel pairs were averaged. Internal R = 0.03
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5784
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.808
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.61
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.273
_refine_ls_abs_structure_details 'Flack H D  (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   14.810
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     307
_refine_ls_number_reflns         2800
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.040
_refine_ls_R_factor_gt           0.032
_refine_ls_shift/esd_mean        0.001
_refine_ls_shift/su_max          0.005
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.672
_refine_ls_wR_factor_ref         0.050
_reflns_number_gt                2800
_reflns_number_total             3263
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            ic010204w.cif
_cod_data_source_block           st717
_cod_original_cell_volume        2515.3(2)
_cod_original_sg_symbol_Hall     ' P 2ac 2ab'
_cod_database_code               4320292