Macrocyclic Complexes of Palladium(II) with Benzothiacrown Ethers: Synthesis, Characterization, and Structure ofcisandtransIsomers
Svetlana N. Dmitrieva; Natalia I. Sidorenko; Nikolay A. Kurchavov; Artem I. Vedernikov; Alexandra Ya. Freidzon; Lyudmila G. Kuz'mina; Aleksei K. Buryak; Tat'yana M. Buslaeva; Alexander A. Bagatur'yants; Yuri A. Strelenko; Judith A. K. Howard; Sergey P. Gromov; Inorganic Chemistry 50 (2011) 7500–7510; doi:10.1021/ic2003063

data_4325848
_publ_section_title
;
 Macrocyclic Complexes of Palladium(II) with Benzothiacrown Ethers:
 Synthesis, Characterization, and Structure ofcisandtransIsomers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7500
_journal_page_last               7510
_journal_paper_doi               10.1021/ic2003063
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C13 H16 Cl2 O3 Pd S2'
_chemical_formula_weight         461.68
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.8827(4)
_cell_length_b                   22.5032(11)
_cell_length_c                   8.8948(5)
_cell_measurement_reflns_used    1663
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.910
_cell_measurement_theta_min      2.462
_cell_volume                     1577.81(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'BRUKER SMART CCD'
_diffrn_measurement_method       /W
_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  0.0615
_diffrn_reflns_av_sigmaI/netI    0.0789
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10103
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    1.784
_exptl_absorpt_correction_T_max  0.7634
_exptl_absorpt_correction_T_min  0.6350
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.944
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.142
_refine_diff_density_min         -1.776
_refine_diff_density_rms         0.146
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         4140
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0391P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.1022
_reflns_number_gt                3210
_reflns_number_total             4140
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2003063_si_002.cif
_cod_data_source_block           5+PdCl2
_cod_database_code               4325848