Walphos versus Biferrocene-Based Walphos Analogues in the Asymmetric Hydrogenation of Alkenes and Ketones.
Zirakzadeh, Afrooz; Groß, Manuela A; Wang, Yaping; Mereiter, Kurt; Weissensteiner, Walter; Organometallics 33 (2014) 1945–1952; doi:10.1021/om401074a

data_4082968
_publ_section_title
;
 Walphos versus Biferrocene-Based Walphos Analogues in the Asymmetric
 Hydrogenation of Alkenes and Ketones.
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1945
_journal_page_last               1952
_journal_paper_doi               10.1021/om401074a
_journal_volume                  33
_journal_year                    2014
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C46 H46 B2 Fe2 P2, C H2 Cl2 '
_chemical_formula_sum            'C47 H48 B2 Cl2 Fe2 P2'
_chemical_formula_weight         879.01
_chemical_name_common
'1695 afzi666 (R,S~Fc~,S~Fc~)-2.(BH3)2.CH2Cl2'
_chemical_name_systematic
; 
(S~Fc~)-2-((R)-1-Diphenylphosphinoethyl)-(S~Fc~)-2''-diphenylphosphino-
1,1''-biferrocene P,P'' bis-borane dichloromethane solvate, 
(R,S~Fc~,S~Fc~)-2.(BH3)2.CH2Cl2
;
_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                 93.674(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.3173(3)
_cell_length_b                   9.5521(3)
_cell_length_c                   20.2125(5)
_cell_measurement_reflns_used    9286
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.93
_cell_measurement_theta_min      2.36
_cell_volume                     2180.56(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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 APEX-II 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  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            55105
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.893
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
The crystal contained disordered solvent, dichloromethane overlain
by diethyl ether in ca. 60:40 proportion. Therefore the solvent was 
squeezed with program PLATON (Spek, A.L., 2010). Listed below
are the most prominent solvent peaks identified by procedure
SQUEEZE:

TITL sq1                    R = 0.03
CELL   11.3173    9.5521   20.2125     90.00     93.67     90.00
SPGR P21
C101 0.296 0.567 0.869 !       8.18 eA-3
C102 0.887 0.113 0.050 !       6.11 eA-3
C103 0.249 0.576 0.939 !       4.43 eA-3
C104 0.143 0.574 0.917 !       4.05 eA-3
C105 0.952 0.108 0.016 !       2.97 eA-3
C106 0.972 0.753-0.004 !       1.97 eA-3
C107 0.953 0.587 0.953 !       1.79 eA-3
   Q108 0.545 0.598 0.389 !       1.49 eA-3
   Q109 0.454 0.907 0.593 !       1.31 eA-3
   Q110 0.158 0.991 0.749 !       1.22 eA-3
   Q111 0.456 0.080 0.587 !       1.21 eA-3
   Q112 0.843 0.481 0.217 !       1.01 eA-3
C113 0.689 0.929 0.137 !       0.92 eA-3
   Q114 0.158 0.766 0.787 !       0.79 eA-3
   Q115 0.844 0.253 0.256 !       0.63 eA-3
   Q116 0.453 0.996 0.594 !       0.63 eA-3
   Q117 0.532 0.838 0.613 !       0.57 eA-3
   Q118 0.158 0.233 0.659 !       0.56 eA-3
C119 0.047 0.544 0.036 !       0.51 eA-3
C120 0.097 0.584 0.846 !       0.51 eA-3
;
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.020(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         12614
_refine_ls_number_restraints     285
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0401P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0679
_reflns_number_gt                11510
_reflns_number_total             12614
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om401074a_si_002.cif
_cod_data_source_block           2xBH3-1695
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4082968--4082970.cif.

 Adding full bibliography for 4082968--4082970.cif.
;
_cod_original_sg_symbol_Hall     'P 2yb  '
_cod_original_sg_symbol_H-M      'P 21   '
_cod_database_code               4082968