Binaphthyl Schiff base complexes of palladium(II). Structures and reactivities toward alkene epoxidation
Zhou, Xiang-Ge; Huang, Jie-Sheng; Yu, Xiao-Qi; Zhou, Zhong-Yuan; Che, Chi-Ming; Journal of the Chemical Society, Dalton Transactions  (2000) 1075–; doi:10.1039/a908917i

data_7009143
_publ_section_title
;
 Binaphthyl Schiff base complexes of palladium(II). Structures and
 reactivities toward alkene epoxidation
;
_journal_issue                   7
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1075
_journal_paper_doi               10.1039/a908917i
_journal_year                    2000
_chemical_formula_sum            'C34.5 H19 Cl5 N2 O2 Pd'
_chemical_formula_weight         777.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                63.28(3)
_cell_angle_beta                 71.03(3)
_cell_angle_gamma                75.74(3)
_cell_formula_units_Z            2
_cell_length_a                   10.359(2)
_cell_length_b                   13.218(3)
_cell_length_c                   14.597(3)
_cell_measurement_reflns_used    'OMEGA SCANS'
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     1676.4(8)
_computing_cell_refinement       'SIMENS XSCANS'
_computing_data_collection       'SIMENS XSCANS'
_computing_data_reduction        SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.737
_diffrn_measured_fraction_theta_max 0.737
_diffrn_measurement_device_type  'SIMENS P4'
_diffrn_measurement_method       'OMEGA SCANS'
_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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0820
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_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5104
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.81
_diffrn_standards_decay_%        1.62
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.986
_exptl_absorpt_correction_T_max  0.8909
_exptl_absorpt_correction_T_min  0.8123
_exptl_absorpt_correction_type   SEMI-EMPIRICAL
_exptl_crystal_colour            BLACK
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             774
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.961
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       0.0000(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_ref   1.165
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         4846
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0733
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1925
_refine_ls_wR_factor_ref         0.1997
_reflns_number_gt                4118
_reflns_number_total             4846
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a908917i.txt
_cod_data_source_block           zx
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1676.4(6)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C34.50 H19 Cl5 N2 O2 Pd'
_cod_database_code               7009143