Chiral, Hemilabile Palladium(II) Complexes of Tridentate Oxazolidines, Including C2-Symmetric "Pincers"
Elizabeth T. J. Strong; Steven A. Cardile; Allison L. Brazeau; Michael C. Jennings; Robert McDonald; Nathan D. Jones; Inorganic Chemistry 47 (2008) 10575–10586; doi:10.1021/ic8011926

data_4306341
_publ_contact_author_address
;
Department of Chemistry
The University of Western Ontario
London, Ontario
CANADA N6A 5B7
;
_publ_contact_author_email       njones26@uwo.ca
_publ_contact_author_fax         '(519) 661-3022'
_publ_contact_author_name        'Dr. Nathan D. Jones'
_publ_contact_author_phone       '(519) 661-2111 ext. 84456'
_publ_section_title
;
Chiral, Hemilabile Palladium(II) Complexes of Tridentate Oxazolidines,
Including C2-Symmetric "Pincers"
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10575
_journal_page_last               10586
_journal_paper_doi               10.1021/ic8011926
_journal_volume                  47
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C27 H31 Cl N3 O2 Pd, F6 P, 0.75(C H2 Cl2)'
_chemical_formula_sum            'C27.75 H32.5 Cl2.5 F6 N3 O2 P Pd'
_chemical_formula_weight         780.06
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'June 26th, 2008'
_audit_creation_method
'from SHELXL97 CIF and IUCr SHELXL97-template'
_audit_update_record             '  compilation of CIF files'
_cell_angle_alpha                90.00
_cell_angle_beta                 117.2795(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.8608(16)
_cell_length_b                   9.9054(6)
_cell_length_c                   27.5099(17)
_cell_measurement_reflns_used    6309
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.38
_cell_measurement_theta_min      2.24
_cell_volume                     6263.2(7)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-96 (Beurskens et al., 1996)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0162
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            27663
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.924
_exptl_absorpt_correction_T_max  0.7818
_exptl_absorpt_correction_T_min  0.6208
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3148
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.28
_platon_squeeze_details
;

 Attempts to refine peaks of residual electron density as disordered or

 partial-occupancy solvent dichloromethane chlorine or carbon atoms were

 unsuccessful.  The data were corrected for disordered electron density

 through use of the SQUEEZE procedure (Sluis, P. van der; Spek, A. L. Acta

 Crystallogr. 1990, A46, 194-201) as implemented in PLATON (Spek, A.L. Acta

 Crystallogr. 1990, A46, C34.  PLATON - a multipurpose crystallographic

 tool.  Utrecht University, Utrecht, The Netherlands).  A total

 solvent-accessible void volume of 675.0 \%A^3^ with a total electron count

 of 263 (consistent with six molecules of solvent dichloromethane, or 0.75

 molecule per formula unit of the palladium complex ion) was found in the

 unit cell.

;
_refine_diff_density_max         1.234
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.012(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         14218
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0527P)^2^+7.7955P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0910
_reflns_number_gt                13449
_reflns_number_total             14218
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic8011926_si_003_2.cif
_cod_data_source_block           8maj.0.75CH2Cl2
_cod_depositor_comments
;
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               4306341