Optically active cyclopalladated derivatives of arylimines. Crystal structures of (+)-[{Pd[p-MeOC6H3CHNCH2-(1S,2R,5S)CHCH2CH2CHC(Me)2CHCH2](μ-X)}2] (X = Cl or Br), (+)-[Pd{p-MeOC6H3CHNCH2-(1S,2R,5S )-CHCH2CH2CHC(Me)2CHCH2}Cl(PPh3)] and (+)-[{Pd[p-MeOC6H3CHNCH2-(1S,2R,5S)-CHCH2CH2CHC(Me)2CHCH2]Cl}2{Fe(δ5-C5H4PPh2)2}]
Zhao, Gang; Wang, Qi-Guang; Mak, Thomas C. W.; Journal of the Chemical Society, Dalton Transactions  (1998) 1241–; doi:10.1039/a708407b

data_7027897
_publ_section_title
;
 Optically active cyclopalladated derivatives of arylimines. Crystal
 structures of
 (+)-[{P&#xE010;d[p-MeOC6H3CH&#xE006;N&#xE011;CH2-(1S,2R,5S)C&#xE010;HCH2CH2C&#xE012;HC(Me)2C&#xE011;HC&#xE013;H2](\m-X)}2]
 (X&#x2005;=&#x2005;Cl or Br),
 (+)-[P&#xE010;d{p-MeOC6H3CH&#xE006;N&#xE011;CH2-(1S,2R,5S&#x200A;)-C&#xE010;HCH2CH2C&#xE012;HC(Me)2C&#xE011;HC&#xE013;H2}Cl(PPh3)]
 and
 (+)-[{P&#xE010;d[p-MeOC6H3CH&#xE006;N&#xE011;CH2-(1S,2R,5S)-C&#xE010;HCH2CH2C&#xE012;HC(Me)2C&#xE011;HC&#xE013;H2]Cl}2{Fe(\d5-C5H4PPh2)2}]
;
_journal_issue                   7
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1241
_journal_paper_doi               10.1039/a708407b
_journal_year                    1998
_chemical_formula_sum            'C35.5 H38 Br Cl Fe0.5 N O P Pd'
_chemical_formula_weight         775.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 90.70(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.730(3)
_cell_length_b                   16.415(3)
_cell_length_c                   25.250(5)
_cell_measurement_temperature    293(2)
_cell_volume                     6934(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0624
_diffrn_reflns_av_sigmaI/netI    0.0784
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            20315
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    2.040
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_F_000             3136
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.08(2)
_refine_ls_extinction_coef       0.00220(8)
_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   1.108
_refine_ls_goodness_of_fit_obs   1.142
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1514
_refine_ls_number_reflns         12092
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.136
_refine_ls_restrained_S_obs      1.142
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_obs          0.0694
_refine_ls_shift/esd_max         0.055
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0889P)^2^+5.1309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1797
_refine_ls_wR_factor_obs         0.1667
_reflns_number_observed          10414
_reflns_number_total             12097
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b708407sup1.cif
_cod_data_source_block           zgb17
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0889P)^2^+5.1309P] 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^)+(0.0889P)^2^+5.1309P] 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        6933.7(22)
_cod_original_formula_sum        'C35.50 H38 Br Cl Fe0.50 N O P Pd'
_cod_database_code               7027897