Designer cyclopalladated-amine catalysts for the asymmetric Claisen rearrangement
Leung, Pak-Hing; Ng, Khim-Hui; Li, Yongxin; White, Andrew J. P.; Williams, David J.; Chemical Communications  (1999) 2435–; doi:10.1039/a907617d

data_7115237
_publ_section_title
;
 Designer cyclopalladated-amine catalysts for the asymmetric Claisen
 rearrangement
;
_journal_issue                   23
_journal_name_full               'Chemical Communications'
_journal_page_first              2435
_journal_paper_doi               10.1039/a907617d
_journal_year                    1999
_chemical_formula_sum            'C22 H24.5 Cl N3 O4.25 Pd'
_chemical_formula_weight         540.80
_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                 108.603(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.399(2)
_cell_length_b                   7.6006(7)
_cell_length_c                   13.0976(11)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.50
_cell_measurement_theta_min      4.66
_cell_volume                     1169.8(2)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3005
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.97
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.941
_exptl_absorpt_correction_T_max  0.8635
_exptl_absorpt_correction_T_min  0.7529
_exptl_absorpt_correction_type   'Face-indexed numerical'
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       prisms
_exptl_crystal_F_000             549
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.031
_refine_ls_goodness_of_fit_obs   1.051
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         2832
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_restrained_S_obs      1.051
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_obs          0.0321
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0795
_refine_ls_wR_factor_obs         0.0768
_reflns_number_observed          2628
_reflns_number_total             2879
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            907617d.txt
_cod_data_source_block           HG9901
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.0000P] 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^)+(0.0396P)^2^+0.0000P] 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_original_formula_sum        'C22 H24.50 N3 O4.25 Cl Pd'
_cod_database_code               7115237