Synthesis, Coordination Behavior, and Structural Features of Chiral Amino-, Pyrazolyl-, and Phosphino-Substituted Ferrocenyloxazolines and Their Application in Asymmetric Hydrogenations
Schuecker, Raffael; Zirakzadeh, Afrooz; Mereiter, Kurt; Spindler, Felix; Weissensteiner, Walter; Organometallics 30 (2011) 4711–; doi:10.1021/om200557c

data_4065090
_publ_section_title
;
 Synthesis, Coordination Behavior, and Structural Features of Chiral
 Amino-, Pyrazolyl-, and Phosphino-Substituted Ferrocenyloxazolines and
 Their Application in Asymmetric Hydrogenations
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4711
_journal_paper_doi               10.1021/om200557c
_journal_volume                  30
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C43 H44 Cl Fe N O P Ru, F6 P, C H Cl3 '
_chemical_formula_sum            'C44 H45 Cl4 F6 Fe N O P2 Ru'
_chemical_formula_weight         1078.47
_chemical_name_common
;
1460 RASC448/449 (R~Ru~)-[RuCl(p-cymene)((4R,1'R,R~Fc~)-19)]PF~6~.CHCl~3~
;
_chemical_name_systematic
; 
(R~Ru~)-Chloro[(4R,1'R,R~Fc~)-2-(4,5-dihydro-4-phenyloxazol-2-yl-\kN)-
1-[1-(diphenylphosphino)ethyl-\kP]-ferrocene-N,P](\n6-p-cymene)ruthenium 
hexafluorophosphate chlroform solvate
;
_space_group_IT_number           1
_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                114.932(2)
_cell_angle_beta                 97.005(2)
_cell_angle_gamma                98.421(2)
_cell_formula_units_Z            1
_cell_length_a                   9.9046(3)
_cell_length_b                   10.6630(3)
_cell_length_c                   11.8693(4)
_cell_measurement_reflns_used    6321
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      3.08
_cell_volume                     1100.65(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT, SADABS, XPREP'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker Smart APEX 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  0.0146
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13153
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.050
_exptl_absorpt_correction_T_max  0.68
_exptl_absorpt_correction_T_min  0.53
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'program SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             546
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.024(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         8041
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0195
_refine_ls_R_factor_gt           0.0193
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+0.2021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0497
_refine_ls_wR_factor_ref         0.0500
_reflns_number_gt                7977
_reflns_number_total             8041
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200557c_si_002.cif
_cod_data_source_block           RuClpc-RRR19
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1100.64(6)
_cod_original_sg_symbol_H-M      P1
_cod_database_code               4065090