A Bidentate Bisphosphine Functioning in Intramolecular Aliphatic Metalation and as an NMR Spectroscopic Probe for the Metal Coordination Environment
William Lesueur; Euro Solari; Carlo Floriani; Angiola Chiesi-Villa; Corrado Rizzoli; Inorganic Chemistry 36 (1997) 3354–3362; doi:10.1021/ic9700819

data_4323510
_publ_contact_author
;
     Dr. Corrado Rizzoli
     Universit\'a di Parma
     Dipartimento di Chimica Generale ed Inorganica,
     Chimica Analitica, Chimica Fisica
     Viale delle Scienze 78
     I-43100 Parma
     Italy
;
_publ_contact_author_email       rizzoli@at@ipruniv.cce.unipr.it
_publ_contact_author_fax         '[039]521 905 556'
_publ_contact_author_phone       '[039]521 905 449'
_publ_section_title
;
 A Bidentate Bisphosphine Functioning in Intramolecular Aliphatic
 Metalation and as an NMR Spectroscopic Probe for the Metal Coordination
 Environment
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3354
_journal_page_last               3362
_journal_paper_doi               10.1021/ic9700819
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C51 H45 Cl P2 Pd'
_chemical_formula_weight         861.72
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                91.20(1)
_cell_angle_beta                 110.27(1)
_cell_angle_gamma                105.26(1)
_cell_formula_units_Z            2.00
_cell_length_a                   11.289(1)
_cell_length_b                   18.769(2)
_cell_length_c                   11.077(1)
_cell_measurement_reflns_used    295
_cell_measurement_temperature    25
_cell_measurement_theta_max      39.5
_cell_measurement_theta_min      29.2
_cell_volume                     2107.7(4)
_computing_cell_refinement       'Belletti et al., 1993'
_computing_data_collection       'Belletti, Cantoni & Pasquinell'
_computing_data_reduction        'DIFAU (Belletti et al.)'
_computing_structure_refinement  'SHELXS-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-76 (Sheldrick, 1976)'
_diffrn_ambient_temperature      295
_diffrn_measurement_device       'Siemens AED'
_diffrn_measurement_method       theta/2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         fine-focus_sealed_tube
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8033
_diffrn_reflns_theta_max         69.95
_diffrn_reflns_theta_min         4.29
_diffrn_standards_decay_%        1.1
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.2104
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.590
_exptl_absorpt_correction_type   'ABSORB: F. Ugozzoli 1987'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.3578
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             888.0
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.22
_refine_diff_density_max         .666
_refine_diff_density_min         -.627
_refine_diff_density_rms         .056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.021
_refine_ls_goodness_of_fit_obs   1.021
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         6155
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_restrained_S_obs      1.121
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_obs          0.0387
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0678P)^2^+0.3196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1124
_refine_ls_wR_factor_obs         0.1025
_reflns_number_observed          6155
_reflns_number_total             8004
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9700819_4.cif
_cod_data_source_block           COMPLEX12
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' 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^)+(0.0678P)^2^+0.3196P] 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^)+(0.0678P)^2^+0.3196P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        C51H45ClP2Pd
_cod_database_code               4323510