Modular syntheses of chiral and achiral C,N-chelated Pd(ii)-pyridinylidenes
Strong, Elizabeth T. J.; Price, Jacquelyn T.; Jones, Nathan D.; Dalton Transactions  (2009) 9123–; doi:10.1039/b915085d

data_7002609
_publ_section_title
;
 Modular syntheses of chiral and achiral C,N-chelated
 Pd(ii)-pyridinylidenes
;
_journal_issue                   42
_journal_name_full               'Dalton Transactions'
_journal_page_first              9123
_journal_paper_doi               10.1039/b915085d
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_formula_sum            'C29 H30 F6 N6 O6 Pd S2'
_chemical_formula_weight         843.11
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.968(3)
_cell_length_b                   13.049(3)
_cell_length_c                   22.681(5)
_cell_measurement_reflns_used    55219
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.04
_cell_volume                     3838.1(15)
_computing_cell_refinement       'Bruker SMART (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SMART (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SMART (Bruker, 1997)'
_computing_publication_material  'Bruker SMART (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full .999
_diffrn_measured_fraction_theta_max .999
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            8748
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.667
_exptl_absorpt_correction_T_max  0.8951
_exptl_absorpt_correction_T_min  0.7024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle/plate
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.17
_refine_diff_density_max         .616
_refine_diff_density_min         -.988
_refine_diff_density_rms         .109
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         8748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0805P)^2^+4.7287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1393
_reflns_number_gt                7888
_reflns_number_total             8748
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b915085d.txt
_cod_data_source_block           7
_cod_original_cell_volume        3838.0(13)
_cod_database_code               7002609