Syntheses, Structural Aspects, Solution Behavior, and Catalytic Utility of CyclopalladatedN,N′,N″-Triarylguanidines [κ2(C,N))Pd(Pyrazole)2X] (X = Br, OC(O)CF3, and PF6) in Suzuki‒Miyaura Coupling Reactions of Aryl Bromides
Agarwal, Pallavi; Thirupathi, Natesan; Nethaji, Munirathinam; Organometallics 35 (2016) 3112–; doi:10.1021/acs.organomet.6b00442

data_4086709
_publ_section_title
;
 Syntheses, Structural Aspects, Solution Behavior, and Catalytic Utility
 of CyclopalladatedN,N&#x2032;,N&#x2033;-Triarylguanidines
 [\k2(C,N))Pd(Pyrazole)2X] (X = Br, OC(O)CF3, and PF6) in Suzuki--Miyaura
 Coupling Reactions of Aryl Bromides
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              3112
_journal_paper_doi               10.1021/acs.organomet.6b00442
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C32 H38 F6 N7 P Pd'
_chemical_formula_sum            'C32 H38 F6 N7 P Pd'
_chemical_formula_weight         772.06
_chemical_melting_point          436.9
_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                 93.959(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9960(15)
_cell_length_b                   19.6317(14)
_cell_length_c                   13.8257(10)
_cell_measurement_reflns_used    6227
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      2.9
_cell_volume                     3519.0(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'
_computing_publication_material  'WINGX V1.80.01'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_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
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_sigmaI/netI    0.0502
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31033
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.637
_exptl_absorpt_correction_T_max  0.9628
_exptl_absorpt_correction_T_min  0.8778
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CRYSALISPRO 1.171.34.49 (2011)'
_exptl_crystal_colour            WHITE
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       HEXAGONAL
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.023
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         7205
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.1112
_refine_ls_R_factor_gt           0.0890
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0680P)^2^+8.6228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1902
_refine_ls_wR_factor_ref         0.2010
_reflns_number_gt                5843
_reflns_number_total             7205
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00442_si_002.cif
_cod_data_source_block           14
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'MONOCLINIC' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/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/current/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 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4086709