Nickel(II) and Palladium(II) Thiaethyneporphyrins. Intramolecular Metal(II)-η2-CC Interaction inside a Porphyrinoid Frame
Elżbieta Nojman; Anna Berlicka; Ludmiła Szterenberg; Lechosław Latos-Grażyński; Inorganic Chemistry 51 (2012) 3247–3260; doi:10.1021/ic2027175

data_4328583
_publ_contact_author_email       lechoslaw.latos-grazynski@chem.uni.wroc.pl
_publ_section_title
;
 Nickel(II) and Palladium(II) Thiaethyneporphyrins. Intramolecular
 Metal(II)-\h2-CC Interaction inside a Porphyrinoid Frame
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3247
_journal_page_last               3260
_journal_paper_doi               10.1021/ic2027175
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C44 H30 N2 Pd S, 1.0(C H Cl3)'
_chemical_formula_sum            'C45 H31 Cl3 N2 Pd S'
_chemical_formula_weight         844.66
_chemical_name_systematic
'palladium(II) 3,18-diphenyl-8,13-di-p-tolyl-20-thiaethyneporphyrin'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 107.995(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.479(6)
_cell_length_b                   8.418(3)
_cell_length_c                   27.478(1)
_cell_measurement_reflns_used    50451
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.5
_cell_measurement_theta_min      0
_cell_volume                     3625.3(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'GONIOMETER OXFORD DIFFRACTION KM4 XCALIBUR2'
_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  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            26742
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         4.44
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.919
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_description       plate
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         7466
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0530P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                6020
_reflns_number_total             7466
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2027175_si_002_3.cif
_cod_data_source_block           noj2
_cod_database_code               4328583