Synthesis and Structural Studies of NCN Diimine Palladium Pincer Complexes Bearingm-Terphenyl Scaffolds
Liqing Ma; Philip M. Imbesi; James B. Updegraff; Allen D. Hunter; John D. Protasiewicz; Inorganic Chemistry 46 (2007) 5220–5228; doi:10.1021/ic062476a

data_4308022
_publ_section_title
;
Synthesis and Structural Studies of NCN Diimine Palladium Pincer Complexes
Bearingm-Terphenyl Scaffolds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5220
_journal_page_last               5228
_journal_paper_doi               10.1021/ic062476a
_journal_volume                  46
_journal_year                    2007
_chemical_absolute_configuration rm
_chemical_formula_sum            'C36 H31 I N2 Pd'
_chemical_formula_weight         724.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           144
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31'
_symmetry_space_group_name_H-M   'P 31'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   15.7499(2)
_cell_length_b                   15.7499(2)
_cell_length_c                   10.5822(2)
_cell_measurement_temperature    100(2)
_cell_volume                     2273.33(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            51541
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    1.658
_exptl_absorpt_correction_T_max  0.7658
_exptl_absorpt_correction_T_min  0.7546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'AXScale in Apex2 (Bruker, 2004)'
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.020(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         7199
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0143
_refine_ls_R_factor_gt           0.0139
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0196P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0335
_refine_ls_wR_factor_ref         0.0336
_reflns_number_gt                7089
_reflns_number_total             7199
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062476a-file001_5.cif
_cod_data_source_block           13a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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_database_code               4308022