Heterobimetallic intermediates in alkene insertion reactions into a Pd‒acetyl bond
Braunstein, Pierre; Durand, Jérôme; Knorr, Michael; Strohmann, Carsten; Chemical Communications  (2001) 211–; doi:10.1039/b007171o

data_7111120
_publ_section_title
;
 Heterobimetallic intermediates in alkene insertion reactions into a
 Pd--acetyl bond
;
_journal_issue                   2
_journal_name_full               'Chemical Communications'
_journal_page_first              211
_journal_paper_doi               10.1039/b007171o
_journal_year                    2001
_chemical_formula_sum            'C33 H31 B Cl2 F4 Fe N O5 P2 Pd'
_chemical_formula_weight         903.49
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.40(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.468(2)
_cell_length_b                   14.540(3)
_cell_length_c                   20.969(4)
_cell_measurement_temperature    173(2)
_cell_volume                     3697.9(13)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Stoe IPDS  '
_diffrn_measurement_method       'image plate'
_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  0.0607
_diffrn_reflns_av_sigmaI/netI    0.0632
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29287
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    1.170
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_F_000             1812
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.862
_refine_diff_density_min         -0.910
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       0.0033(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.001
_refine_ls_goodness_of_fit_obs   1.187
_refine_ls_hydrogen_treatment    'geom, riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         7201
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_restrained_S_obs      1.187
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_obs          0.0573
_refine_ls_shift/esd_max         -0.050
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0899P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1518
_refine_ls_wR_factor_obs         0.1404
_reflns_number_observed          4531
_reflns_number_total             7202
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b007171osup1.cif
_cod_data_source_block           5a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0899P)^2^+0.0000P] 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^)+(0.0899P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3697.9(12)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7111120