The palladium(II) complex of N,N-diethyl-1-ferrocenyl-3-thiabutanamine: synthesis, solution and solid state structure and catalytic activity in Suzuki-Miyaura reaction
Damljanovic, Ivan; Stevanovic, Dragana; Pejovic, Anka; Ilic, Danijela; Zivkovic, Marija; Jovanovic, Jovana; Vukicevic, Mirjana; Radulović, Niko S; Bogdanovic, Goran A.; Vukicevic, Rastko D.; RSC Adv.  (2014) –; doi:10.1039/C4RA08140D

data_7217847
_publ_section_title
;
 The palladium(II) complex of N,N-diethyl-1-ferrocenyl-3-thiabutanamine:
 synthesis, solution and solid state structure and catalytic activity in
 Suzuki-Miyaura reaction
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA08140D
_journal_year                    2014
_chemical_formula_moiety         'C17 H25 Cl2 Fe N Pd S, C2 H6 O'
_chemical_formula_sum            'C19 H31 Cl2 Fe N O Pd S'
_chemical_formula_weight         554.66
_chemical_name_systematic
;
dichlorido-(N,N-diethyl-1-ferrocenyl-3-thiabutanamine)palladium(II)
;
_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                 105.836(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8670(4)
_cell_length_b                   14.7863(4)
_cell_length_c                   13.4527(6)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.3690
_cell_measurement_theta_min      3.4320
_cell_volume                     2270.94(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;ORTEP3 (Farrugia, 1997,
 Mercury CSD 2.4.5 (Build RC3), CCDC, Cambridge (2011)
;
_computing_publication_material
'WinGX (Farrugia, 1999) and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.3280
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type
;
'Oxford Xcalibur, Sapphire3, Gemini'
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33237
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.68
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    1.766
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         5858
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0273P)^2^+3.6960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1037
_reflns_number_gt                4792
_reflns_number_total             5858
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra08140d2.cif
_cod_data_source_block           polymorph-I
_cod_original_cell_volume        2270.94(14)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7217847