First Resolution of a Free Fluorophosphine Chiral at Phosphorus. Resolution and Reactions of Free and Coordinated (\±)-Fluorophenylisopropylphosphine
Michael Pabel; Anthony C. Willis; S. Bruce Wild; Inorganic Chemistry 35 (1996) 1244–1249; doi:10.1021/ic950897e

data_4323784
_publ_contact_author
;
Dr S. B. Wild
Research School of Chemistry
Australian National University
Canberra A.C.T. 0200
Australia
;
_publ_contact_author_email       ' willis@rsc3.anu.edu.au '
_publ_contact_author_fax         ' 61 6 249 0750 '
_publ_contact_author_phone       ' 61 6 249 4236 '
_publ_section_title
;
 First Resolution of a Free Fluorophosphine Chiral at Phosphorus.
 Resolution and Reactions of Free and Coordinated
 (\+-)-Fluorophenylisopropylphosphine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1244
_journal_page_last               1249
_journal_paper_doi               10.1021/ic950897e
_journal_volume                  35
_journal_year                    1996
_chemical_formula_moiety         'C24 H31 Cl N O P Pd '
_chemical_formula_structural     '(Pd Cl (C14 H16 N) (C10 H15 O P) ) '
_chemical_formula_sum            'C24 H31 Cl N O P Pd'
_chemical_formula_weight         522.34
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_date             'Mon Oct 16 15:08:31 1995'
_audit_creation_method           'from TEXRAY.INF file'
_audit_update_record
;
95.11.03   acw:  cif modified from raw texsan version
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.444(3)
_cell_length_b                   12.146(3)
_cell_length_c                   19.047(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      17.3
_cell_measurement_theta_min      15.4
_cell_volume                     2416.2(10)
_computing_cell_refinement       'Xtal 3.2: LATCON'
_computing_data_collection       'Philips PW1100/20 software 1976'
_computing_data_reduction        'Xtal 3.2: DIFDAT, ABSORB, ADDREF'
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Philips PW1100/20'
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_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       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            4918
_diffrn_reflns_theta_max         25.00
_diffrn_standards_decay_%        2.00
_diffrn_standards_interval_time  180
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.960
_exptl_absorpt_correction_T_max  0.842
_exptl_absorpt_correction_T_min  0.782
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       block
_exptl_crystal_F_000             1072.00
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.27
_refine_diff_density_min         -0.33
_refine_ls_abs_structure_details
;
>From the known chirality of the ligand precursor and comparison of
Friedel opposites.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.540
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         2096
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0260
_refine_ls_shift/esd_max         0.0240
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0290
_reflns_number_observed          2096
_reflns_number_total             2456
_reflns_observed_criterion       3.00
_cod_data_source_file            ic950897e_2.cif
_cod_data_source_block           MXP7_the_methoxide
_cod_original_cell_volume        2416.2(9)
_cod_original_sg_symbol_Hall     'p 2ac 2ab'
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C24 H31 Cl N O P Pd '
_cod_database_code               4323784