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_4328581
_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         'C24 H20 N2'
_chemical_formula_sum            'C24 H20 N2'
_chemical_formula_weight         336.42
_chemical_name_systematic        1,4-diphenyl-1,4-di(pyrrol-2-yl)-but-2-yn
_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                 95.557(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.855(3)
_cell_length_b                   6.835(1)
_cell_length_c                   16.605(4)
_cell_measurement_reflns_used    18928
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      0
_cell_volume                     1791.0(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0804
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14921
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         0
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'transparent brown'
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       plate
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.038
_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     243
_refine_ls_number_reflns         4190
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0291P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0822
_reflns_number_gt                2793
_reflns_number_total             4190
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2027175_si_002_1.cif
_cod_data_source_block           noj21
_cod_original_sg_symbol_Hall     '-P 2ybn'
_cod_database_code               4328581