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_4063787
_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         'C32  H33  Br Cl2  N4  O3  Pd'
_chemical_formula_sum            'C32 H33 Br Cl2 N4 O3 Pd'
_chemical_formula_weight         778.83
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.897(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.268(4)
_cell_length_b                   14.844(7)
_cell_length_c                   21.449(9)
_cell_measurement_reflns_used    698
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.50
_cell_volume                     3257(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    SHELXS-97
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.3
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.1297
_diffrn_reflns_av_sigmaI/netI    0.1931
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22611
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    1.999
_exptl_absorpt_correction_T_max  0.5958
_exptl_absorpt_correction_T_min  0.5140
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       RECTANGULAR
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.081
_refine_diff_density_min         -1.535
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.784
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         9439
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.784
_refine_ls_R_factor_all          0.1982
_refine_ls_R_factor_gt           0.0746
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1012P)^2^+55.0804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2082
_refine_ls_wR_factor_ref         0.2727
_reflns_number_gt                4213
_reflns_number_total             9439
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1009445_si_001.cif
_cod_data_source_block           354_0m1
_cod_depositor_comments
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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 
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_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4063787