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_4066337
_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            'C37 H36 Fe N P3'
_chemical_formula_weight         643.43
_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             2008-08-02T17:27:47-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                99.385(3)
_cell_angle_beta                 97.342(3)
_cell_angle_gamma                108.169(3)
_cell_formula_units_Z            2
_cell_length_a                   10.2115(4)
_cell_length_b                   11.4581(4)
_cell_length_c                   14.7424(6)
_cell_measurement_reflns_used    7867
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      32.2081
_cell_measurement_theta_min      2.6092
_cell_volume                     1587.35(11)
_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_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 16.356
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'ccd xcalibur s'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0451982849
_diffrn_orient_matrix_UB_12      -0.0135320278
_diffrn_orient_matrix_UB_13      0.0323865401
_diffrn_orient_matrix_UB_21      0.0123015133
_diffrn_orient_matrix_UB_22      0.0650939379
_diffrn_orient_matrix_UB_23      0.0151527977
_diffrn_orient_matrix_UB_31      -0.0577688454
_diffrn_orient_matrix_UB_32      -0.0047782546
_diffrn_orient_matrix_UB_33      -0.0343454501
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.0782
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29482
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.99381
_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    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.872
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         6500
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.872
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0288P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0679
_reflns_number_gt                4383
_reflns_number_total             6500
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1004012_si_001.cif
_cod_data_source_block           x0459fin
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4066337