Novel heteroleptic cis-(C-N)2Pd(II) chelates for the preparation of enantiopure planar chiral cyclopalladated 2-[tricarbonyl(eta6-phenyl)chromium]pyridine
Djukic, Jean-Pierre; Alexsandro, Berger; Andre de, Cian; Nathalie, Kyritsakas-Gruber; Jerome, Lacour; Michel, Pfeffer; Laurent, Vial; Chemical communications (Cambridge, England)  (2003) –; doi:10.1039/b211873d

data_7104001
_publ_section_title
;
Novel heteroleptic cis-(C-N)2Pd(II) chelates for the
preparation of enantiopure planar chiral cyclopalladated 
2-[tricarbonyl(eta6-phenyl)chromium]pyridine
;
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/b211873d
_journal_year                    2003
_chemical_formula_moiety         'C20 H15 Cl3 Cr N2 O3 Pd'
_chemical_formula_sum            'C20 H15 Cl3 Cr N2 O3 Pd'
_chemical_formula_weight         596.11
_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'
_cell_angle_alpha                90
_cell_angle_beta                 96.103(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.4747(2)
_cell_length_b                   12.4324(3)
_cell_length_c                   14.0935(5)
_cell_measurement_temperature    173
_cell_volume                     1128.04(6)
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      173
_diffrn_measurement_details
;
6353 reflections were collected using program Collect
("Collect" Data collection software, Nonius B.V., 1998)
The conditions were as follow : crystal to detector distance =  36. mm.
Scan angle =  2.0 deg 1 scans of   50 sec per frame.
Data collection was divided into  2 set(s)
with the following starting angles and number of frames :

Set 1 Theta =    8.80 Omega =    0.00 Kappa =    0.00   90 frames
Set 2 Theta =   -8.50 Kappa = -165.00 Phi   =    0.00   15 frames
Friedel pairs were averaged. Internal R = 0.04
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6353
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.658
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9592
_exptl_absorpt_correction_type   refdelf_(Walker_&_Stuart,_1983)
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.75
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.137
_refine_diff_density_min         -0.866
_refine_ls_abs_structure_details 'Flack H D  (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   13.275
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    12
_refine_ls_number_parameters     255
_refine_ls_number_reflns         2879
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.049
_refine_ls_R_factor_gt           0.040
_refine_ls_shift/esd_mean        0.001
_refine_ls_shift/su_max          0.012
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.663
_refine_ls_wR_factor_ref         0.057
_reflns_number_gt                2879
_reflns_number_total             3451
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            b211873d.txt
_cod_data_source_block           pR3
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_database_code               7104001