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_7002048
_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_formula_moiety         'C34 H31 Cl N2 P Pd, C F3 O3 S, C H2 Cl2 '
_chemical_formula_sum            'C36 H33 Cl3 F3 N2 O3 P Pd S'
_chemical_formula_weight         874.46
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P -2bc -2c'
_symmetry_space_group_name_H-M   'P c 21 b'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             07-06-01
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1808(10)
_cell_length_b                   18.1687(12)
_cell_length_c                   18.3719(13)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    180
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     3732.1(5)
_computing_cell_refinement       'IPDS (Stoe & Cie, 1996)'
_computing_data_collection       'IPDS (Stoe & Cie, 1996)'
_computing_data_reduction        'XRED (Stoe & Cie 1996)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34134
_diffrn_reflns_theta_full        25.482
_diffrn_reflns_theta_max         26.002
_diffrn_reflns_theta_min         2.132
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_description       block
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.53
_refine_diff_density_min         -0.53
_refine_ls_abs_structure_details 'Flack (1983), 3499 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         5127
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.001483
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
1.16 0.477E-02 0.644
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0473
_refine_ls_wR_factor_gt          0.0405
_refine_ls_wR_factor_ref         0.0405
_reflns_limit_h_max              13
_reflns_limit_h_min              0
_reflns_limit_k_max              22
_reflns_limit_k_min              -22
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                5127
_reflns_number_total             7271
_reflns_threshold_expression     I>3.0\s(I)
_cod_data_source_file            b907019b.txt
_cod_data_source_block           CIFnath53
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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_sg_symbol_H-M      'P c 21 b '
_cod_original_formula_sum        'C36 H33 Cl3 F3 N2 O3 P1 Pd1 S1'
_cod_database_code               7002048