Enantiopure planar chiral monomers and di-μ-bromo-bridged dimers of ferrocenylhydrazones from asymmetric cyclopalladation
Zhao, Gang; Wang, Qi-Guang; Mak, Thomas C. W.; Journal of the Chemical Society, Dalton Transactions  (1998) 3785–; doi:10.1039/a806052e

data_7028054
_publ_section_title
;
 Enantiopure planar chiral monomers and di-\m-bromo-bridged dimers of
 ferrocenylhydrazones from asymmetric cyclopalladation
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3785
_journal_paper_doi               10.1039/a806052e
_journal_year                    1998
_chemical_compound_source        synthesized
_chemical_formula_sum            'C48 H58 Br2 Fe2 N4 O2 Pd2'
_chemical_formula_weight         1207.30
_chemical_name_common            syn-(-)-(Sp,S,S,Sp)-5
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   10.651(2)
_cell_length_b                   13.215(3)
_cell_length_c                   34.580(7)
_cell_measurement_temperature    293(2)
_cell_volume                     4867.2(17)
_computing_cell_refinement       BIOTEX
_computing_data_collection       R-AXIS
_computing_data_reduction        BIOTEX
_computing_molecular_graphics    'SIEMENS SHELXL PC'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'RIGAKU RXAIS II'
_diffrn_measurement_method       IP
_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  0.1174
_diffrn_reflns_av_sigmaI/netI    0.1259
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            10974
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    2.994
_exptl_absorpt_correction_type   ABSCOR
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_description       plate
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.354
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.140
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.490(12)
_refine_ls_extinction_coef       0.00079(13)
_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   1.067
_refine_ls_goodness_of_fit_obs   1.082
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         6292
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_restrained_S_obs      1.082
_refine_ls_R_factor_all          0.1049
_refine_ls_R_factor_obs          0.0958
_refine_ls_shift/esd_max         -0.614
_refine_ls_shift/esd_mean        0.033
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1812P)^2^+0.9059P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2590
_refine_ls_wR_factor_obs         0.2468
_reflns_number_observed          5618
_reflns_number_total             6296
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            e806052sup1.cif
_cod_data_source_block           zgf64
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1812P)^2^+0.9059P] 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^)+(0.1812P)^2^+0.9059P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7028054