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_4065087
_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 rm
_chemical_formula_moiety         'C33 H30 Cl2 Fe N O P Pd, 2(C H Cl3)'
_chemical_formula_sum            'C35 H32 Cl8 Fe N O P Pd'
_chemical_formula_weight         959.44
_chemical_name_common
'1452 RASC455 [PdCl~2~((4R,1'R,R~Fc~)-19)].2(CHCl~3~)'
_chemical_name_systematic
; 
Dichloro[(4R,1'R,R~Fc~)-2-(4,5-dihydro-4-phenyloxazol-2-yl)-1-
[1-(diphenylphosphino)ethyl]-ferrocene-N,P]palladium bis(chloroform) solvate 
;
_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                 107.376(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.36350(10)
_cell_length_b                   16.4396(2)
_cell_length_c                   13.0475(2)
_cell_measurement_reflns_used    8097
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      2.48
_cell_volume                     1916.78(4)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0171
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28894
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.477
_exptl_absorpt_correction_T_max  0.63
_exptl_absorpt_correction_T_min  0.51
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'program SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.016(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         10055
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0195
_refine_ls_R_factor_gt           0.0191
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+0.6604P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0479
_refine_ls_wR_factor_ref         0.0481
_reflns_number_gt                9923
_reflns_number_total             10055
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200557c_si_002.cif
_cod_data_source_block           PdCl2-RRR19
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      P2(1)
_cod_database_code               4065087