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_7002050
_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         'C31 H25 Cl2 N2 P Pd, 2(C H2 Cl2)'
_chemical_formula_sum            'C33 H29 Cl6 N2 P Pd'
_chemical_formula_weight         803.70
_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
_audit_creation_date             09-03-27
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90
_cell_angle_beta                 91.664(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6431(4)
_cell_length_b                   12.0659(4)
_cell_length_c                   22.2303(8)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    180
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     3389.8(2)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Bruker Kappa Apex2'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w 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       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            42948
_diffrn_reflns_theta_full        27.938
_diffrn_reflns_theta_max         27.938
_diffrn_reflns_theta_min         0.916
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.094
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, acta cryst. (1995), a51, 33-38'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.68
_refine_diff_density_min         -1.67
_refine_ls_abs_structure_details 'Flack (1983), 7338 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0872
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     746
_refine_ls_number_reflns         11755
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.000572
_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:
1.25 0.226 0.588
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0848
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0639
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                12852
_reflns_number_total             15846
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0588
_oxford_reflns_number_all        15791
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title 'yc230309_0m in P2(1)'
_cod_data_source_file            b907019b.txt
_cod_data_source_block           CIFyc230309
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 1 21 1 '
_cod_original_formula_sum        'C33 H29 Cl6 N2 P1 Pd1'
_cod_database_code               7002050