Hydrocarbyl derivatives of dppm- or dppa-bridged alkoxysilyl heterobimetallic Fe‒Pd complexes and CO insertion reactions. Crystal structures of [(OC)3{(MeO)3Si}Fe(μ-dppm)Pd(8-mq)] (dppm = Ph2PCH2PPh2), [(OC)3Fe{μ-Si(OMe)2(OMe)}(μ-dppa)PdCl] and [(OC)3Fe{μ-Si(OMe)2(OMe)}(μ-dppa)PdPh] (dppa = Ph2PNHPPh2) †
Braunstein, Pierre; Durand, Jérôme; Kickelbick, Guido; Knorr, Michael; Morise, Xavier; Pugin, Raphael; Tiripicchio, Antonio; Ugozzoli, Franco; Journal of the Chemical Society, Dalton Transactions  (1999) 4175–; doi:10.1039/a907425b

data_7027802
_publ_section_title
;
 Hydrocarbyl derivatives of dppm- or dppa-bridged alkoxysilyl
 heterobimetallic Fe--Pd complexes and CO insertion reactions. Crystal
 structures of [(OC)3{(MeO)3Si}&#xE010;Fe(\m-dppm)P&#xE011;d(8-mq)]
 (dppm&#x2005;=&#x2005;Ph2PCH2PPh2),
 [(OC)3&#xE010;Fe{\m-Si(OMe)2(&#xE012;OMe)}(\m-dppa)P&#xE013;&#xE011;dCl]
 and
 [(OC)3&#xE010;Fe{\m-Si(OMe)2(&#xE012;OMe)}(\m-dppa)P&#xE013;&#xE011;dPh]
 (dppa&#x2005;=&#x2005;Ph2PNHPPh2)&#x200A;&#x2020;
;
_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4175
_journal_paper_doi               10.1039/a907425b
_journal_year                    1999
_chemical_formula_sum            'C30 H30 Cl Fe N O6 P2 Pd Si'
_chemical_formula_weight         788.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_space_group_name_Hall  '-P 3*'
_symmetry_space_group_name_H-M   'R -3 :R'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                118.39(2)
_cell_angle_beta                 118.39(2)
_cell_angle_gamma                118.39(2)
_cell_formula_units_Z            6
_cell_length_a                   25.113(2)
_cell_length_b                   25.113(2)
_cell_length_c                   25.113(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    298
_cell_measurement_theta_max      18
_cell_measurement_theta_min      13
_cell_volume                     5176(18)
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298
_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  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            14457
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    1.187
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_F_000             2388
_refine_diff_density_max         1.020
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.169
_refine_ls_extinction_coef       0.00000(15)
_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   1.389
_refine_ls_goodness_of_fit_obs   0.899
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         4503
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.389
_refine_ls_restrained_S_obs      0.899
_refine_ls_R_factor_all          0.1309
_refine_ls_R_factor_obs          0.0316
_refine_ls_shift/esd_max         1.684
_refine_ls_shift/esd_mean        0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+27.7168P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1271
_refine_ls_wR_factor_obs         0.0629
_reflns_number_observed          2796
_reflns_number_total             4503
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            907425bsup1.cif
_cod_data_source_block           br88
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+27.7168P] 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^)+(0.0001P)^2^+27.7168P] where P=(Fo^2^+2Fc^2^)/3'.

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

2018-03-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C90 H90 Cl3 Fe3 N3 O18 P6 Pd3 Si3'
_cod_original_formula_weight         2364.84
_cod_original_formula_units_Z            2
_cod_original_cell_volume        5175.8(8)
_cod_database_code               7027802