Modular Approach to Novel Chiral Aryl-Ferrocenyl Phosphines by Suzuki Cross-Coupling
Jakob F. Jensen; Inger Søtofte; Henning O. Sørensen; Mogens Johannsen; Journal of Organic Chemistry 68 (2003) 1258–1265; doi:10.1021/jo026250a

data_4022290
_publ_contact_author_address
;
Department of Chemistry, Building 207
Technical University Denmark
DK-2800 Kgs.Lyngby
Denmark
;
_publ_contact_author_email       mj@kemi.dtu.dk
_publ_contact_author_fax         (+45)45883136
_publ_contact_author_name        'Mogens Johannsen'
_publ_contact_author_phone       (+45)45252027
_publ_section_title
;
 Modular Approach to Novel Chiral Aryl-Ferrocenyl Phosphines
 by Suzuki Cross-Coupling
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1258
_journal_page_last               1265
_journal_paper_doi               10.1021/jo026250a
_journal_volume                  68
_journal_year                    2003
_chemical_formula_sum            'C28 H23 Fe O2 P'
_chemical_formula_weight         478.28
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.45(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.009(2)
_cell_length_b                   12.086(2)
_cell_length_c                   9.979(2)
_cell_measurement_temperature    120(2)
_cell_volume                     1085.5(4)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement
'Siemens SHELXTL PC version 5.3 (Sheldrick, 1994)'
_computing_structure_solution
'Siemens SHELXTL PC version 5.3 (Sheldrick, 1994)'
_diffrn_ambient_temperature      120(2)
_diffrn_measurement_device       'Siemens SMART CCD Platform'
_diffrn_measurement_method       'Omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0523
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7628
_diffrn_reflns_theta_max         29.60
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_count no
_diffrn_standards_interval_time  no
_diffrn_standards_number         no
_exptl_absorpt_coefficient_mu    0.792
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8062
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.023(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.043
_refine_ls_goodness_of_fit_obs   1.057
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5273
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_restrained_S_obs      1.057
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_obs          0.0392
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+0.0353P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0935
_refine_ls_wR_factor_obs         0.0897
_reflns_number_observed          4739
_reflns_number_total             5273
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            jo026250asi20021125_041220.cif
_cod_data_source_block           jf4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'no' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+0.0353P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+0.0353P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4022290