Depalladation of Neutral Monoalkyne- and Dialkyne-Inserted Palladacycles and Alkyne Insertion/Depalladation Reactions of Cationic Palladacycles Derived fromN,N′,N″-Triarylguanidines as Facile Routes for Guanidine-Containing Heterocycles/Carbocycles: Synthetic, Structural, and Mechanistic Aspects
Saxena, Priya; Thirupathi, Natesan; Nethaji, Munirathinam; Organometallics 33 (2014) 5554–; doi:10.1021/om500837v

data_4084412
_publ_contact_author             'Thirupathi N.'
_publ_section_title
;
 Depalladation of Neutral Monoalkyne- and Dialkyne-Inserted Palladacycles
 and Alkyne Insertion/Depalladation Reactions of Cationic Palladacycles
 Derived fromN,N&#x2032;,N&#x2033;-Triarylguanidines as Facile Routes for
 Guanidine-Containing Heterocycles/Carbocycles: Synthetic, Structural, and
 Mechanistic Aspects
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5554
_journal_paper_doi               10.1021/om500837v
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C42 H37 N3 O7'
_chemical_formula_sum            'C42 H37 N3 O7'
_chemical_formula_weight         695.75
_chemical_name_systematic
;
 ?
;
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_cell_angle_beta                 110.329(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
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_cell_length_c                   16.1050(11)
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_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      3.02
_cell_volume                     3702.8(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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
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_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
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_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
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_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.086
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_exptl_absorpt_correction_T_min  0.9666
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrysAlisPro 1.171.34.40 (2006)'
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       IRREGULAR
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_refine_ls_extinction_method     none
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_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0584
_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^)+(0.0929P)^2^+1.1816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1629
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_reflns_number_gt                6357
_reflns_number_total             7566
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om500837v_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'MONOCLINIC' changed to 'monoclinic'
according to
/home/saulius/struct/COD-crude-data--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
/home/saulius/struct/COD-crude-data--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 4084410--4084417.cif.
;
_cod_original_cell_volume        3702.8(4)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4084412