Secondary Ferrocenyl Phosphines: Versatile Precursors for the Synthesis of Bi- and Tridentate Ligands
Buergler, Jonas F.; Togni, Antonio; Organometallics 30 (2011) 4742–; doi:10.1021/om200574k

data_4065127
_publ_section_title
;
 Secondary Ferrocenyl Phosphines: Versatile Precursors for the Synthesis
 of Bi- and Tridentate Ligands
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4742
_journal_paper_doi               10.1021/om200574k
_journal_volume                  30
_journal_year                    2011
_chemical_absolute_configuration rm
_chemical_formula_moiety
'2(C48 H49 Cl F6 Fe2 P3 Pd), 2(F6 P), C Cl2,3(C H2 Cl2)'
_chemical_formula_sum            'C50 H52 Cl5 F12 Fe2 P4 Pd'
_chemical_formula_weight         1400.14
_chemical_melting_point          ?
_chemical_name_systematic
; 
 ? 
;
_chemical_properties_physical    loss_of_solvent
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      1
_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                80.834(2)
_cell_angle_beta                 82.089(2)
_cell_angle_gamma                64.800(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2973(11)
_cell_length_b                   13.4782(12)
_cell_length_c                   18.4298(16)
_cell_measurement_reflns_used    7184
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.71
_cell_measurement_theta_min      2.23
_cell_volume                     2720.3(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0716
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23266
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    1.294
_exptl_absorpt_correction_T_max  0.7264
_exptl_absorpt_correction_T_min  0.6426
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS-2004/1
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1406
_exptl_crystal_recrystallization_method CH2Cl2/hexane
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.773
_refine_diff_density_min         -1.263
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.012(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1333
_refine_ls_number_reflns         19715
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0837P)^2^+2.4305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1451
_reflns_number_gt                18089
_reflns_number_total             19715
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200574k_si_001.cif
_cod_data_source_block           compound15
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P1
_cod_database_code               4065127