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_7028053
_publ_section_title
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 Enantiopure planar chiral monomers and di-\m-bromo-bridged dimers of
 ferrocenylhydrazones from asymmetric cyclopalladation
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_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            'C36 H46 Br2 Fe2 N4 O2 Pd2'
_chemical_formula_weight         1051.09
_chemical_name_common            syn-(-)-(Sp,R,R,Sp)-5
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_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                 96.370(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.8720(10)
_cell_length_b                   11.2960(10)
_cell_length_c                   13.3370(10)
_cell_measurement_temperature    293(2)
_cell_volume                     1927.3(3)
_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  0.0609
_diffrn_reflns_av_sigmaI/netI    0.0645
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6579
_diffrn_reflns_theta_max         25.54
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    3.766
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_description       plate
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.982
_refine_diff_density_min         -1.108
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.641(6)
_refine_ls_extinction_coef       0.0256(5)
_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   1.004
_refine_ls_goodness_of_fit_obs   1.006
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         6457
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.016
_refine_ls_restrained_S_obs      1.006
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_obs          0.0551
_refine_ls_shift/esd_max         1.566
_refine_ls_shift/esd_mean        0.020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1178P)^2^+0.4703P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1586
_refine_ls_wR_factor_obs         0.1555
_reflns_number_observed          6337
_reflns_number_total             6458
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            e806052sup1.cif
_cod_data_source_block           zgf65
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1178P)^2^+0.4703P] 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^)+(0.1178P)^2^+0.4703P] 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)
_cod_database_code               7028053