Mono- and Dialkyne Insertion Reactions of CyclopalladatedN,N′,N″-Triarylguanidines [κ2(C,N)Pd(μ-Br)]2andcis-/trans-[κ2(C,N)Pd(Lewis Base)Br]. Scaffolds for Enlarged, Rearranged, and Zwitterionic Palladacycles through Ring Contraction cum Amine‒Imine Tautomerization
Saxena, Priya; Thirupathi, Natesan; Nethaji, Munirathinam; Organometallics 33 (2014) 3182–; doi:10.1021/om500423q

data_4083575
_publ_contact_author             'Thirupathi N.'
_publ_section_title
;
 Mono- and Dialkyne Insertion Reactions of
 CyclopalladatedN,N&#x2032;,N&#x2033;-Triarylguanidines
 [\k2(C,N)Pd(\m-Br)]2andcis-/trans-[\k2(C,N)Pd(Lewis Base)Br]. Scaffolds
 for Enlarged, Rearranged, and Zwitterionic Palladacycles through Ring
 Contraction cum Amine--Imine Tautomerization
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3182
_journal_paper_doi               10.1021/om500423q
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C44 H42 Br N3 O4 Pd'
_chemical_formula_sum            'C44 H42 Br N3 O4 Pd'
_chemical_formula_weight         863.12
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.464(4)
_cell_angle_beta                 104.639(3)
_cell_angle_gamma                95.510(3)
_cell_formula_units_Z            2
_cell_length_a                   10.5265(4)
_cell_length_b                   13.9731(6)
_cell_length_c                   14.8358(5)
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.87
_cell_volume                     1951.43(15)
_computing_cell_refinement       'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'OLEX 2-2.1'
_computing_publication_material  'WINGX V1.80.01'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 0.3703
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Sapphire-3 CCD detector'
_diffrn_measurement_method       'OMEGA SCAN'
_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  0.0585
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27175
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    1.546
_exptl_absorpt_correction_T_max  0.7273
_exptl_absorpt_correction_T_min  0.6986
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrysAlisPro 1.171.34.40 (2006)'
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       IRREGULAR
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         7965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+0.7117P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0947
_reflns_number_gt                6759
_reflns_number_total             7965
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om500423q_si_002.cif
_cod_data_source_block           1g
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'TRICLINIC' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'EMPIRICAL'
changed to 'empirical' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4083571--4083582.cif.
;
_cod_original_cell_volume        1951.42(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4083575