Atropochiral (C,C)-chelating NHC-ylide ligands: synthesis and resolution of palladium(ii) complexes thereof
Abdellah, Ibrahim; Debono, Nathalie; Canac, Yves; Duhayon, Carine; Chauvin, Remi; Dalton Transactions  (2009) 7196–; doi:10.1039/b907019b

data_7002051
_publ_section_title
;
 Atropochiral (C,C)-chelating NHC-ylide ligands: synthesis and
 resolution of palladium(ii) complexes thereof
;
_journal_issue                   35
_journal_name_full               'Dalton Transactions'
_journal_page_first              7196
_journal_paper_doi               10.1039/b907019b
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C41 H39 N3 P Pd, C F3 O3 S, C H2 Cl2'
_chemical_formula_sum            'C43 H41 Cl2 F3 N3 O3 P Pd S'
_chemical_formula_weight         945.12
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_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
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2369(2)
_cell_length_b                   16.1127(3)
_cell_length_c                   20.5946(4)
_cell_measurement_reflns_used    21225
_cell_measurement_temperature    180
_cell_measurement_theta_max      32.1628
_cell_measurement_theta_min      2.5813
_cell_measurement_wavelength     0.71073
_cell_volume                     4060.63(13)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       \w-\f
_diffrn_orient_matrix_UB_11      0.0069741731
_diffrn_orient_matrix_UB_12      -0.0353284822
_diffrn_orient_matrix_UB_13      0.0201333243
_diffrn_orient_matrix_UB_21      -0.0136936515
_diffrn_orient_matrix_UB_22      0.0241078777
_diffrn_orient_matrix_UB_23      0.0276113995
_diffrn_orient_matrix_UB_31      -0.0558667734
_diffrn_orient_matrix_UB_32      -0.0103354517
_diffrn_orient_matrix_UB_33      -0.0043026446
_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  0.0437
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            44953
_diffrn_reflns_theta_full        32.26
_diffrn_reflns_theta_max         32.26
_diffrn_reflns_theta_min         2.59
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.84332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.27 (release 29-05-2008 CrysAlis171 .NET)
(compiled May 29 2008,13:12:44)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.39
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.026(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         13649
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.063
_refine_ls_wR_factor_ref         0.0669
_reflns_number_gt                10620
_reflns_number_total             13649
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b907019b.txt
_cod_data_source_block           publiyc080908
_cod_database_code               7002051