Thermodynamics and Mechanism of the Reversible Tin-to-Palladium Transmetalation of the Furyl Group
W. Donald Cotter; Lauren Barbour; Kristin L. McNamara; Rachel Hechter; Rene J. Lachicotte; Journal of the American Chemical Society 120 (1998) 11016–11017; doi:10.1021/ja980901w

data_4116858
_publ_section_title
;
 Thermodynamics and Mechanism of the Reversible Tin-to-Palladium
 Transmetalation of the Furyl Group
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11016
_journal_page_last               11017
_journal_paper_doi               10.1021/ja980901w
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C36 H30 O P2 Pd'
_chemical_formula_weight         646.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.7964(2)
_cell_length_b                   15.6983(2)
_cell_length_c                   22.36270(10)
_cell_measurement_temperature    193(2)
_cell_volume                     5896.48(11)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0172
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            34250
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    NA
_exptl_crystal_description       Cluster
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.128
_refine_ls_goodness_of_fit_obs   1.151
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         7049
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_restrained_S_obs      1.151
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_obs          0.0306
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+4.6626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0724
_refine_ls_wR_factor_obs         0.0701
_reflns_number_observed          6382
_reflns_number_total             7049
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja980901w.cif
_cod_data_source_block           pbca
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'NA' 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^)+(0.0292P)^2^+4.6626P] 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^)+(0.0292P)^2^+4.6626P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4116858