New atropisomeric N‒N ligands for CO/vinyl arene copolymerization reaction
Durand, Jérôme; Zangrando, Ennio; Carfagna, Carla; Milani, Barbara; Dalton Transactions  (2008) 2171–2182; doi:10.1039/b716656g

data_7003490
_publ_section_title
;
 New atropisomeric N--N ligands for CO/vinyl arene copolymerization
 reaction
;
_journal_issue                   16
_journal_name_full               'Dalton Transactions'
_journal_page_first              2171
_journal_page_last               2182
_journal_paper_doi               10.1039/b716656g
_journal_year                    2008
_chemical_formula_moiety         'C28 H28 N4 O4 Pd 2+, 2(P F6 1-)'
_chemical_formula_sum            'C28 H28 F12 N4 O4 P2 Pd'
_chemical_formula_weight         880.88
_chemical_name_common
;
bis-((S,S)-3,3-(2,3-butylenedioxy))-2,2-bipyridine)-
palladium(ii) bis(hexafluorophosphate)
;
_chemical_name_systematic
;
bis-[(S,S)-3,3-(2,3-butylenedioxy)]-2,2-bipyridine)-palladium(II)
bis(hexafluorophosphate)
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.89(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.438(3)
_cell_length_b                   10.834(4)
_cell_length_c                   16.503(4)
_cell_measurement_temperature    293(2)
_cell_volume                     1671.5(9)
_computing_cell_refinement       'Mosflm (Acta Cryst. D50, 760, 1994)'
_computing_data_collection       'Nonius Xpress'
_computing_data_reduction        'Scala (Acta Cryst. D50, 760, 1994)'
_computing_molecular_graphics    'Ortep3/windows (Farrugia,1997)'
_computing_publication_material  'Wingx 1.70.00 (Farrugia, 1999)'
_computing_structure_refinement  'SHELX97 (Sheldrick, 1998)'
_computing_structure_solution    'SHELX97 (Sheldrick, 1998)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'image plate dip1030'
_diffrn_measurement_method       'laser scanner'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mok\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0561
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17414
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_T_max  0.9134
_exptl_absorpt_correction_T_min  0.5881
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             880
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         6437
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+0.8580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1140
_reflns_number_gt                5558
_reflns_number_total             6437
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b716656g.txt
_cod_data_source_block           2c
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7003490