Unexpected 1,5-Dilithiation of Chiral o-TMS Blocked (Dimethylamino)phenylmethylferrocene: An Alternative Approach to Chiral Ferrocenyl 1,5-Diphosphanes
Shin-ichi Fukuzawa; Masahisa Yamamoto; Satoshi Kikuchi; Journal of Organic Chemistry 72 (2007) 1514–1517; doi:10.1021/jo062210l

data_4022705
_publ_section_title
;
 Unexpected 1,5-Dilithiation of Chiral o-TMS Blocked
 (Dimethylamino)phenylmethylferrocene: An Alternative
 Approach to Chiral Ferrocenyl 1,5-Diphosphanes
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1514
_journal_page_last               1517
_journal_paper_doi               10.1021/jo062210l
_journal_volume                  72
_journal_year                    2007
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C43 H39 Fe N P2 '
_chemical_formula_sum            'C43 H39 Fe N P2'
_chemical_formula_weight         687.58
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_date             2006-09-28
_audit_creation_method           'by CrystalStructure 3.7.0'
_cell_angle_alpha                90.0000
_cell_angle_beta                 98.07(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   11.807(13)
_cell_length_b                   16.361(15)
_cell_length_c                   18.45(3)
_cell_measurement_reflns_used    169
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      1.7
_cell_volume                     3528(8)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    'DIRDIF99 (PATTY)'
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.898
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32655
_diffrn_reflns_theta_full        31.70
_diffrn_reflns_theta_max         31.70
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_T_max  0.848
_exptl_absorpt_correction_T_min  0.620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1440.00
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.85
_refine_diff_density_min         -0.65
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  6088 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.007(9)
_refine_ls_extinction_coef       82(10)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     927
_refine_ls_number_reflns         12602
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.0043
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[0.0002Fo^2^ + 1.3770\s(Fo^2^)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0392
_reflns_number_gt                12602
_reflns_number_total             17163
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo062210lsi20061025_121101.cif
_cod_data_source_block           '__20060928-2'
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C43 H39 Fe N P2 '
_cod_database_code               4022705