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_4328582
_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 H32 N2 S'
_chemical_formula_sum            'C44 H32 N2 S'
_chemical_formula_weight         620.78
_chemical_name_systematic
3,18-diphenyl-8,13-ditolyl-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                 95.155(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7800(3)
_cell_length_b                   8.2440(2)
_cell_length_c                   28.0630(5)
_cell_measurement_reflns_used    56001
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.55
_cell_measurement_theta_min      0
_cell_volume                     3175.13(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0872
_diffrn_reflns_av_sigmaI/netI    0.1426
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            54497
_diffrn_reflns_theta_full        38.55
_diffrn_reflns_theta_max         38.55
_diffrn_reflns_theta_min         4.22
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       plate
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         17549
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1462
_refine_ls_R_factor_gt           0.0642
_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^)+(0.0392P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1303
_reflns_number_gt                8042
_reflns_number_total             17549
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2027175_si_002_2.cif
_cod_data_source_block           noje
_cod_database_code               4328582