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_4066336
_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_absolute_configuration ad
_chemical_formula_sum            'C39 H40 Fe N O2 P3'
_chemical_formula_weight         703.48
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_audit_creation_date             2009-10-15T15:55:16-00:00
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8067(3)
_cell_length_b                   16.4070(5)
_cell_length_c                   17.0077(4)
_cell_measurement_reflns_used    5342
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      28.8496
_cell_measurement_theta_min      2.9418
_cell_volume                     3573.65(16)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.49 (release 25-09-2009 CrysAlis171 .NET)
        (compiled Sep 25 2009,16:18:01)
;
_computing_data_collection
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        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.49 (release 25-09-2009 CrysAlis171 .NET)
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_computing_data_reduction
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        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.49 (release 25-09-2009 CrysAlis171 .NET)
        (compiled Sep 25 2009,16:18:01)
;
_computing_molecular_graphics
;
 ORTEP3 for Windows
 L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565.
;
_computing_publication_material
;
 WINGX
 L.J. Farrugia,
 J. Appl. Cryst., 1999, 32, 837-838.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
 SIR92
 A. Altomare, G. Cascarano, C. Giacovazzo and A. Guagliardi,
 J. Appl. Crystallogr. 1993, 26, 343-350.
;
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.036196174
_diffrn_orient_matrix_UB_12      0.0212095771
_diffrn_orient_matrix_UB_13      0.0242403769
_diffrn_orient_matrix_UB_21      -0.0194955205
_diffrn_orient_matrix_UB_22      -0.0376926647
_diffrn_orient_matrix_UB_23      0.014191933
_diffrn_orient_matrix_UB_31      0.0371435845
_diffrn_orient_matrix_UB_32      0.0008108481
_diffrn_orient_matrix_UB_33      0.0309619547
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0989
_diffrn_reflns_limit_h_max       16
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_diffrn_reflns_theta_full        26.37
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_exptl_absorpt_coefficient_mu    0.591
_exptl_absorpt_correction_T_max  1
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_exptl_absorpt_process_details
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.49 (release 25-09-2009 CrysAlis171 .NET)
        (compiled Sep 25 2009,16:18:01)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal platelet'
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.26
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.788
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         7294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.788
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0148P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0475
_refine_ls_wR_factor_ref         0.05
_reflns_number_gt                5065
_reflns_number_total             7294
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1004012_si_001.cif
_cod_data_source_block           x0851fin
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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)2(1)2(1)
_cod_database_code               4066336