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_7104000
_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         'C48 H44 Cr2 N4 O6 Pd2'
_chemical_formula_sum            'C48 H44 Cr2 N4 O6 Pd2'
_chemical_formula_weight         1089.70
_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                 102.140(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.1267(2)
_cell_length_b                   17.0317(3)
_cell_length_c                   11.5572(2)
_cell_measurement_temperature    173
_cell_volume                     2141.19(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
;
10295 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 =  1.6 deg 1 scans of   60 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 =  -80.00 Phi   =    0.00   27 frames
Friedel pairs were averaged. Internal R = 0.03
;
_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  0.030
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10295
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.376
_exptl_absorpt_correction_T_max  1.1570
_exptl_absorpt_correction_T_min  0.9783
_exptl_absorpt_correction_type   refdelf_(Walker_&_Stuart,_1983)
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.69
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.117
_refine_ls_abs_structure_details 'Flack H D  (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   9.351
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     558
_refine_ls_number_reflns         5557
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.032
_refine_ls_R_factor_gt           0.023
_refine_ls_shift/esd_mean        0.001
_refine_ls_shift/su_max          0.005
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.279
_refine_ls_wR_factor_ref         0.028
_reflns_number_gt                5557
_reflns_number_total             6443
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            b211873d.txt
_cod_data_source_block           5c
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_database_code               7104000