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_4323783
_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         'C23 H28 Cl F N P Pd '
_chemical_formula_structural     ' ( Pd Cl (C14 H16 N) (C9 H12 F P) ) '
_chemical_formula_sum            'C23 H28 Cl F N P Pd'
_chemical_formula_weight         510.31
_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 15:07:03 1995'
_audit_creation_method           'from TEXRAY.INF file'
_audit_update_record
;
95.11.03  acw modifies raw texsan cif
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.967(2)
_cell_length_b                   10.998(4)
_cell_length_c                   21.324(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298.2
_cell_measurement_theta_max      18.8
_cell_measurement_theta_min      15.6
_cell_volume                     2337.5(10)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      298.2
_diffrn_measurement_device       AFC6S
_diffrn_measurement_method       'omega scans'
_diffrn_orient_matrix_UB_11      0.09092
_diffrn_orient_matrix_UB_12      0.03833
_diffrn_orient_matrix_UB_13      0.00180
_diffrn_orient_matrix_UB_21      0.00307
_diffrn_orient_matrix_UB_22      0.00231
_diffrn_orient_matrix_UB_23      -0.04686
_diffrn_orient_matrix_UB_31      -0.04233
_diffrn_orient_matrix_UB_32      0.08242
_diffrn_orient_matrix_UB_33      0.00049
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.00
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2385
_diffrn_reflns_theta_max         25.03
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.993
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   Coppens_numerical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       block
_exptl_crystal_F_000             1040.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.37
_refine_diff_density_min         -0.46
_refine_ls_abs_structure_details
;
>From the known chirality of the ligand precursor 
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   2.090
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         1528
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0310
_refine_ls_shift/esd_max         0.0140
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0200
_reflns_number_observed          1528
_reflns_number_total             2385
_reflns_observed_criterion       3.00
_cod_data_source_file            ic950897e_1.cif
_cod_data_source_block           MXP3_the_fluoride
_cod_original_cell_volume        2337.3(7)
_cod_original_sg_symbol_Hall     ' p 2ac 2ab '
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C23 H28 Cl F N P Pd '
_cod_database_code               4323783