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_7002049
_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         'C41 H39 N3 P Pd, C F3 O3 S, (H2 O)'
_chemical_formula_sum            'C42 H41 F3 N3 O4 P Pd S'
_chemical_formula_weight         878.24
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_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
_audit_creation_date             08-05-23
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4645(4)
_cell_length_b                   15.7229(4)
_cell_length_c                   20.4721(6)
_cell_measurement_reflns_used    9855
_cell_measurement_temperature    180
_cell_measurement_theta_max      34
_cell_measurement_theta_min      2
_cell_volume                     4012.1(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 0.997
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device       'Bruker apex2'
_diffrn_measurement_device_type  Serial
_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  0.020
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            37731
_diffrn_reflns_theta_full        33.270
_diffrn_reflns_theta_max         35.021
_diffrn_reflns_theta_min         1.633
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.91
_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    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.64
_refine_diff_density_min         -1.45
_refine_ls_abs_structure_details 'Flack (1983), 7053 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0550
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         13663
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.001727
_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:
1.01 0.140 0.655
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0445
_refine_ls_wR_factor_gt          0.0410
_refine_ls_wR_factor_ref         0.0400
_reflns_limit_h_max              20
_reflns_limit_h_min              -19
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                14510
_reflns_number_total             16125
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0363
_oxford_reflns_number_all        16125
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            b907019b.txt
_cod_data_source_block           CifYC190508
_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 21 21 21 '
_cod_original_formula_sum        'C42 H41 F3 N3 O4 P1 Pd1 S1'
_cod_database_code               7002049