Coordination and hydrogen-bonding assemblies in hybrid reaction products between 5,10,15,20-tetra-4-pyridylporphyrin and dysprosium trinitrate hexahydrate
Lipstman, Sophia; Goldberg, Israel; Acta Crystallographica Section C 66 (2010) m222–m226; doi:10.1107/S0108270110026892

data_2017752
_publ_section_title
;
 Coordination and hydrogen-bonding assemblies in hybrid reaction
 products between 5,10,15,20-tetra-4-pyridylporphyrin and dysprosium
 trinitrate hexahydrate
;
_journal_coeditor_code           GD3355
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m222
_journal_page_last               m226
_journal_paper_doi               10.1107/S0108270110026892
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Dy2 (N O3)8 (C40 H28 N8) (H2 O)2], C6 H6'
_chemical_formula_moiety         'C34 H26 Dy2 N16 O26, C6 H6'
_chemical_formula_sum            'C40 H32 Dy2 N16 O26'
_chemical_formula_weight         1477.82
_chemical_name_systematic
;
[\m-5,15-bis(pyridin-1-ium-4-yl)-10,20-di-4-
pyridylporphyrin]bis[aquatetranitratodysprosium(III)] benzene solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.1447(10)
_cell_angle_beta                 89.3410(10)
_cell_angle_gamma                75.3827(16)
_cell_formula_units_Z            1
_cell_length_a                   7.7897(2)
_cell_length_b                   12.2577(2)
_cell_length_c                   17.2316(5)
_cell_measurement_reflns_used    4507
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.09
_cell_measurement_theta_min      1.41
_cell_volume                     1492.45(6)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
ORTEP-III (Burnett & Johnson, 1996),
Mercury (Macrae <i>et al.</i>, 2006)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1994)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 12.8
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. \f and \w scans'
_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  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0818
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13999
_diffrn_reflns_theta_full        27.09
_diffrn_reflns_theta_max         27.09
_diffrn_reflns_theta_min         1.83
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.576
_exptl_absorpt_correction_T_max  0.8820
_exptl_absorpt_correction_T_min  0.6986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.363
_refine_diff_density_min         -1.028
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6457
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0346P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0833
_reflns_number_gt                5074
_reflns_number_total             6457
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gd3355.cif
_cod_data_source_block           I
_cod_database_code               2017752
_cod_database_fobs_code          2017752