Synthesis of Racemic Aminoalkylferrocenyldichlorophosphanes and -dialkylphosphonites and Their Conversion to Primary Phosphanes†
Limburg, Carolin; Lönnecke, Peter; Gómez-Ruiz, Santiago; Hey-Hawkins, Evamarie; Organometallics 29 (2010) 5427–; doi:10.1021/om1004012

data_4066335
_publ_section_title
;
 Synthesis of Racemic Aminoalkylferrocenyldichlorophosphanes and
 -dialkylphosphonites and Their Conversion to Primary Phosphanes&#x2020;
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5427
_journal_paper_doi               10.1021/om1004012
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C46 H56 Fe N O2 P3'
_chemical_formula_weight         803.68
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2008-12-03T12:19:42-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                93.855(2)
_cell_angle_beta                 102.631(2)
_cell_angle_gamma                111.892(3)
_cell_formula_units_Z            2
_cell_length_a                   10.0395(2)
_cell_length_b                   10.9011(3)
_cell_length_c                   22.0156(5)
_cell_measurement_reflns_used    14915
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      32.264
_cell_measurement_theta_min      2.555
_cell_volume                     2151.92(10)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
;
_computing_molecular_graphics    'ORTEP3 for Windows (L. J. Farrugia, 1997)'
_computing_publication_material  'WINGX  (L.J. Farrugia,1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo 1993)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 16.356
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'ccd Xcalibur S'
_diffrn_measurement_method       \w-scans
_diffrn_orient_matrix_UB_11      0.0007470116
_diffrn_orient_matrix_UB_12      -0.0627067731
_diffrn_orient_matrix_UB_13      0.0062132906
_diffrn_orient_matrix_UB_21      -0.0681094941
_diffrn_orient_matrix_UB_22      -0.0332974437
_diffrn_orient_matrix_UB_23      -0.0234798923
_diffrn_orient_matrix_UB_31      0.0395696176
_diffrn_orient_matrix_UB_32      0.0000521962
_diffrn_orient_matrix_UB_33      -0.0229927202
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            36205
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    0.499
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.99839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.24
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.593
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         13085
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0735P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1284
_reflns_number_gt                9101
_reflns_number_total             13085
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1004012_si_001.cif
_cod_data_source_block           x0652fin
_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        2151.92(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4066335