Redetermination of <i>cyclo</i>-tetrakis(μ-5,10,15,20-tetra-4-pyridylporphyrinato)tetrazinc(II) dimethylformamide octasolvate trihydrate at 100K
Seidel, Rüdiger W.; Graf, Jürgen; Goddard, Richard; Oppel, Iris M.; Acta Crystallographica Section E 67 (2011) m236–m237; doi:10.1107/S1600536811002054

data_2228989
_publ_section_title
;
 Redetermination of
 <i>cyclo</i>-tetrakis(\m-5,10,15,20-tetra-4-pyridylporphyrinato)tetrazinc(II)
 dimethylformamide octasolvate trihydrate at 100K
;
_journal_coeditor_code           BV2170
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m236
_journal_page_last               m237
_journal_paper_doi               10.1107/S1600536811002054
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Zn4 (C40 H24 N8)4], 8C3 H7 N O, 3H2 O'
_chemical_formula_moiety         'C160 H96 N32 Zn4, 8(C3 H7 N O), 3(H2 O)'
_chemical_formula_sum            'C184 H158 N40 O11 Zn4'
_chemical_formula_weight         3366.98
_chemical_name_systematic
;
<i>cyclo</i>-tetrakis(\m-5,10,15,20-tetra-4-pyridylporphyrinato)tetrazinc(II)
dimethylformamide octasolvate
;
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   23.6897(5)
_cell_length_b                   23.6897(5)
_cell_length_c                   14.9876(7)
_cell_measurement_reflns_used    130
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      3.5
_cell_volume                     8411.1(5)
_computing_cell_refinement       'SAINT (Bruker, 2010)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2010)'
_computing_publication_material  'enCIFer (Allen <i>et al.</i>, 2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker X8 PROSPECTOR goniometer'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Incoatec Quazar Multilayer Mirror'
_diffrn_radiation_source         'Incoatec I\mS microfocus X-ray source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0183
_diffrn_reflns_av_sigmaI/netI    0.0129
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            44415
_diffrn_reflns_theta_full        69.17
_diffrn_reflns_theta_max         69.17
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    1.238
_exptl_absorpt_correction_T_max  0.9757
_exptl_absorpt_correction_T_min  0.8265
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3500
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.421
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7723
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+5.0454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1075
_reflns_number_gt                6768
_reflns_number_total             7723
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            bv2170.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               2228989
_cod_database_fobs_code          2228989