1H NMR Investigation of High-Spin and Low-Spin Iron(III)meso-Ethynylporphyrins
Anna Berlicka; Lechosław Latos-Grażyński; Tadeusz Lis; Inorganic Chemistry 44 (2005) 4522–4533; doi:10.1021/ic050158q

data_4309087
_publ_section_title
;
1H NMR Investigation of High-Spin and Low-Spin
Iron(III)meso-Ethynylporphyrins
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4522
_journal_page_last               4533
_journal_paper_doi               10.1021/ic050158q
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C94 H74 N8 O2 Zn2'
_chemical_formula_sum            'C94 H74 N8 O2 Zn2'
_chemical_formula_weight         1478.35
_chemical_name_systematic
;
1,4-bis-[10,15,20-tri(p-tolyl)porphyrin-5-yl]-1,3-butadiyne
;
_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                 104.54(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.092(3)
_cell_length_b                   13.529(3)
_cell_length_c                   18.244(3)
_cell_measurement_reflns_used    16264
_cell_measurement_temperature    100(2)
_cell_volume                     3605.8(13)
_computing_cell_refinement
'CrysAlis RED (Oxford Diffraction, 1995-2003)'
_computing_data_collection
'CrysAlis CCD (Oxford Diffraction, 1995-2003)'
_computing_data_reduction
'CrysAlis RED (Oxford Diffraction, 1995-2003)'
_computing_molecular_graphics    'XP (Bruker, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'KUMA KM4 CCD \k-geometry diffractometer'
_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  0.0521
_diffrn_reflns_av_sigmaI/netI    0.0717
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29240
_diffrn_reflns_theta_full        28.45
_diffrn_reflns_theta_max         28.45
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    0.725
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.834
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'CrysAlis RED(Oxford Diffraction, 1995-2003)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.731
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         8521
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0870P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_gt          0.1401
_refine_ls_wR_factor_ref         0.1539
_reflns_number_gt                5783
_reflns_number_total             8521
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050158qsi20050131_110352_2.cif
_cod_data_source_block           dimer
_cod_original_cell_volume        3605.7(12)
_cod_database_code               4309087