Intermolecular iodine‒iodine interactions in bis(pyridine-3-carboxylato)[tetrakis(4-iodophenyl)porphyrinato]tin(IV) and bis(pyrimidine-5-carboxylato)[tetrakis(4-iodophenyl)porphyrinato]tin(IV)
Titi, Hatem M.; Patra, Ranjan; Goldberg, Israel; Acta Crystallographica Section C 69 (2013) 1013–1016; doi:10.1107/S0108270113020209

data_2019128
_publ_section_title
;
 Intermolecular iodine--iodine interactions in
 bis(pyridine-3-carboxylato)[tetrakis(4-iodophenyl)porphyrinato]tin(IV)
 and
 bis(pyrimidine-5-carboxylato)[tetrakis(4-iodophenyl)porphyrinato]tin(IV)
;
_journal_coeditor_code           FG3302
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1013
_journal_page_last               1016
_journal_paper_doi               10.1107/S0108270113020209
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac
'[Sn (C44 H24 I4 N4) (C6 H4 N O2)2] , 1.5C3 H7 N O'
_chemical_formula_moiety         'C56 H32 I4 N6 O4 Sn, 1.5(C3 H7 N O)'
_chemical_formula_sum            'C60.5 H42.5 I4 N7.5 O5.5 Sn'
_chemical_formula_weight         1558.81
_chemical_name_systematic
;
bis(pyridine-3-carboxylato)[tetrakis(4-iodophenyl)porphyrinato]tin(IV)
dimethylformamide sesquisolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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           SHELXL2012
_cell_angle_alpha                90
_cell_angle_beta                 98.1460(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.0594(3)
_cell_length_b                   17.1924(3)
_cell_length_c                   11.4740(2)
_cell_measurement_reflns_used    4946
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.85
_cell_measurement_theta_min      2.15
_cell_volume                     2745.45(9)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material  'SHELXL2012 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL2012 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 12.8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1\% \f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11339
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.855
_diffrn_reflns_theta_min         2.149
_exptl_absorpt_coefficient_mu    2.774
_exptl_absorpt_correction_T_max  0.733
_exptl_absorpt_correction_T_min  0.491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.922
_exptl_crystal_description       plate
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.120
_platon_squeeze_details
;
The 61 electrons removed from the two sites around 0.5, 1.0, 0.0 and
0.5, 0.5, 0.5 would correspond to 1.5 molecules of the DMF solvent (which has
40 electrons) at each site. This suggests that three molecules of DMF per
unit cell (1.5 molecules per porphyrin unit) are entrapped in the crystal
lattice.
;
_refine_diff_density_max         1.842
_refine_diff_density_min         -0.878
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         6485
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0690P)^2^+0.2949P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1098
_reflns_number_gt                4946
_reflns_number_total             6485
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg3302.cif
_cod_data_source_block           I
_cod_database_code               2019128
_cod_database_fobs_code          2019128
_shelx_estimated_absorpt_t_min   0.491
_shelx_estimated_absorpt_t_max   0.733
_shelx_res_checksum              32496
_shelxl_version_number           .000002012