Chiral and Stable Palladium(0) Complexes of Polyunsaturated Aza-macrocyclic Ligands: Synthesis and Structural Analysis
Pla-Quintana, Anna; Torrent, Anna; Dachs, Anna; Roglans, Anna; Pleixats, Roser; Moreno-Mañas, Marcial; Parella, Teodor; Benet-Buchholz, Jordi; Organometallics 25 (2006) 5612–; doi:10.1021/om060667f

data_4074472
_publ_contact_author
;
    Dr. Benet-Buchholz, Jordi
    Institute of Chemical Research of Catalonia (ICIQ)    
    X-ray Diffraction Unit
    Avgda. Pa\=isos Catalans 16
    E-43007 Tarragona, Spain
;
_publ_section_title
;
 Chiral and Stable Palladium(0) Complexes of Polyunsaturated
 Aza-macrocyclic Ligands:&#x00A0; Synthesis and Structural Analysis
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              5612
_journal_paper_doi               10.1021/om060667f
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C55.25 H65.5 Cl0.5 N5 O10 Pd S5'
_chemical_formula_weight         1244.05
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.293(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.677(3)
_cell_length_b                   29.570(5)
_cell_length_c                   13.074(2)
_cell_measurement_reflns_used    5278
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.77
_cell_measurement_theta_min      2.77
_cell_volume                     6322.5(18)
_computing_cell_refinement       'Bruker-Nonius Apex v1.0-22 2002'
_computing_data_collection       'Bruker-Nonius Apex v1.0-22 2002'
_computing_data_reduction        'SAINT+ Version 7.06A Bruker-Nonius, 2004'
_computing_molecular_graphics    'Shelxtl Version 6.12 (Sheldrick, 2001)'
_computing_publication_material  'Shelxtl Version 6.12 (Sheldrick, 2001)'
_computing_structure_refinement  'Shelxtl Version 6.12 (Sheldrick, 2001)'
_computing_structure_solution    'Shelxtl Version 6.12 (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 0.849
_diffrn_measured_fraction_theta_max 0.849
_diffrn_measurement_device_type  'Kappa 4-axis goniometer bruker-nonius'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support
'magnetic support whith 10 micron nylon fiber cryoloop'
_diffrn_radiation_monochromator  'Multilayer Montel 200 mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1400
_diffrn_reflns_av_sigmaI/netI    0.1905
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            73941
_diffrn_reflns_theta_full        36.41
_diffrn_reflns_theta_max         36.41
_diffrn_reflns_theta_min         2.77
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_current           90
_diffrn_source_power             50
_diffrn_source_size              '3 mm x 0.3 mm fine focus'
_diffrn_source_type              'Bruker-Nonius FR 591'
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7469
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS Version 2.1 2003 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2586
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.290
_refine_diff_density_min         -3.048
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     812
_refine_ls_number_reflns         26196
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.2033
_refine_ls_R_factor_gt           0.0874
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1427P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2132
_refine_ls_wR_factor_ref         0.2766
_reflns_number_gt                12016
_reflns_number_total             26196
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060667fsi20060726_061000.cif
_cod_data_source_block           ap353e
_cod_depositor_comments
;
The following automatic conversions were performed:
'_diffrn_measurement_specimen_suppport' tag replaced with
'_diffrn_measurement_specimen_support'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        6323(2)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C55.25 H65.50 Cl0.50 N5 O10 Pd S5'
_cod_database_code               4074472