Aminoalkylferrocenyldichlorophosphanes: facile synthesis of versatile chiral starting materials.
Tschirschwitz, Steffen; Lönnecke, Peter; Hey-Hawkins, Evamarie; Dalton transactions (Cambridge, England : 2003)  (2007) 1377–1382; doi:10.1039/b617257a

data_7005159
_publ_section_title
;
 Aminoalkylferrocenyldichlorophosphanes: facile synthesis of versatile
 chiral starting materials.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1377
_journal_page_last               1382
_journal_paper_doi               10.1039/b617257a
_journal_year                    2007
_chemical_formula_sum            'C37 H44 Cl2 Fe N P Si'
_chemical_formula_weight         688.54
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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             2006-11-14T12:23:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 95.2190(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.29870(10)
_cell_length_b                   21.9790(2)
_cell_length_c                   14.68120(10)
_cell_measurement_reflns_used    32151
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      32.2282
_cell_measurement_theta_min      2.6828
_cell_volume                     3309.39(5)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 16.356
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'ccd xcalibur s'
_diffrn_measurement_method       '\w scans and \f scans'
_diffrn_orient_matrix_UB_11      -0.0036132007
_diffrn_orient_matrix_UB_12      0.0317572015
_diffrn_orient_matrix_UB_13      -0.0076322812
_diffrn_orient_matrix_UB_21      0.028396904
_diffrn_orient_matrix_UB_22      -0.003807979
_diffrn_orient_matrix_UB_23      -0.041842872
_diffrn_orient_matrix_UB_31      -0.0629361235
_diffrn_orient_matrix_UB_32      -0.0035572133
_diffrn_orient_matrix_UB_33      -0.0233075638
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            49152
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.69
_exptl_absorpt_coefficient_mu    0.73
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.83904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.54
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         9966
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0471P)^2^+2.1585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1042
_reflns_number_gt                8304
_reflns_number_total             9966
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b617257a.txt
_cod_data_source_block           x0062fin
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7005159