Synthesis, Reactivity, Structural Aspects, and Solution Dynamics of Cyclopalladated Compounds ofN,N′,N′′-Tris(2-anisyl)guanidine
Gopi, Kanniyappan; Thirupathi, Natesan; Nethaji, Munirathinam; Organometallics 30 (2011) 572–; doi:10.1021/om1009445

data_4063784
_publ_section_title
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 Synthesis, Reactivity, Structural Aspects, and Solution Dynamics of
 Cyclopalladated Compounds
 ofN,N&#x2032;,N&#x2032;&#x2032;-Tris(2-anisyl)guanidine
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_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              572
_journal_paper_doi               10.1021/om1009445
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C50 H56 BR2 N6 O8 PD2'
_chemical_formula_sum            'C50 H56 Br2 N6 O8 Pd2'
_chemical_formula_weight         1241.63
_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                 96.078(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.432(5)
_cell_length_b                   10.795(5)
_cell_length_c                   22.836(10)
_cell_measurement_reflns_used    698
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.50
_cell_volume                     2557(2)
_computing_cell_refinement       'BRUKER SMART APEX CCD'
_computing_data_collection       'BRUKER SMART APEX CCD'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    ORTEP-III
_computing_publication_material  'WINGX V1.64.05'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHLXS-97
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean .3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device_type  'BRUKER SMART APEX CCD'
_diffrn_measurement_method       OMEGA
_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  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            21643
_diffrn_reflns_theta_full        27.75
_diffrn_reflns_theta_max         27.75
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    2.323
_exptl_absorpt_correction_T_max  0.5532
_exptl_absorpt_correction_T_min  0.4835
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS'
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       RECTANGULAR
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     312
_refine_ls_number_reflns         6026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0742P)^2^+2.1593P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1224
_reflns_number_gt                4577
_reflns_number_total             6026
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1009445_si_001.cif
_cod_data_source_block           pnt289_m
_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.

'_exptl_absorpt_correction_type' value 'EMPIRICAL'
changed to 'empirical' 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        2557.2(19)
_cod_original_sg_symbol_H-M      P21/C
_cod_database_code               4063784