Synthesis of Ferrocenyl Diphosphine Ligands: Substitution of α-Methoxy or α-Dimethylamino Groups by Phosphines. Retention versus Inversion: A Stereochemical Study
Schuecker, Raffael; Weissensteiner, Walter; Mereiter, Kurt; Lotz, Matthias; Spindler, Felix; Organometallics 29 (2010) 6443–; doi:10.1021/om100843u

data_4067132
_publ_section_title
;
 Synthesis of Ferrocenyl Diphosphine Ligands: Substitution of \a-Methoxy
 or \a-Dimethylamino Groups by Phosphines. Retention versus Inversion: A
 Stereochemical Study
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6443
_journal_paper_doi               10.1021/om100843u
_journal_volume                  29
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C48 H38 Cl2 F12 Fe P2 Pd Si, C H Cl3'
_chemical_formula_sum            'C49 H39 Cl5 F12 Fe P2 Pd Si'
_chemical_formula_weight         1285.33
_chemical_name_common            '1346 [PdCl2((R,S~Fc~)-3b)].CHCl~3~'
_chemical_name_systematic
; 
Dichloro[(R,S~Fc~)-1-trimethylsilyl-2-
[\a-(bis(3,5-bistrifluoromethylphenyl))phosphino-\kP)-
(2-diphenylphosphinophenyl)methyl-\kP]-ferrocene-P,P] palladium
trichloromethane solvate, [PdCl2((R,S~Fc~)-3b)].CHCl~3~
;
_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                 95.214(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.7270(16)
_cell_length_b                   13.3092(19)
_cell_length_c                   18.395(3)
_cell_measurement_reflns_used    7595
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.37
_cell_measurement_theta_min      2.44
_cell_volume                     2615.3(7)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            44338
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.038
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'program SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.103
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.022(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         15197
_refine_ls_number_restraints     271
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0584P)^2^+1.5383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1138
_reflns_number_gt                12647
_reflns_number_total             15197
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100843u_si_001.cif
_cod_data_source_block           PdCl2RSfc-3b
_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               4067132