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_2017753
_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
'(C40 H30 N8) [Dy (N O3)2 (H2 O)5] (N O3)5, 2C2 H6 O, 2H2 O'
_chemical_formula_moiety
'C40 H30 N8 4+, Dy H10 N2 O11 +, 5(N O3 -), 2(C2 H6 O), 2(H2 O)'
_chemical_formula_sum            'C44 H56 Dy N15 O30'
_chemical_formula_weight         1437.54
_chemical_name_systematic
;
5,10,15,20-tetrakis(pyridin-1-ium-4-yl)porphyrin
pentaaquadinitratodysprosate(III) pentanitrate diethanol solvate dihydrate
;
_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                71.6843(7)
_cell_angle_beta                 80.9684(8)
_cell_angle_gamma                73.3707(7)
_cell_formula_units_Z            2
_cell_length_a                   12.8961(2)
_cell_length_b                   12.9222(2)
_cell_length_c                   18.5978(3)
_cell_measurement_reflns_used    12265
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      1.41
_cell_volume                     2811.52(8)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. \f & \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  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            47169
_diffrn_reflns_theta_full        27.86
_diffrn_reflns_theta_max         27.86
_diffrn_reflns_theta_min         2.31
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.438
_exptl_absorpt_correction_T_max  0.9316
_exptl_absorpt_correction_T_min  0.5119
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1462
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.000
_refine_diff_density_min         -1.616
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     813
_refine_ls_number_reflns         13315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+2.8440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0817
_reflns_number_gt                11865
_reflns_number_total             13315
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gd3355.cif
_cod_data_source_block           II
_cod_database_code               2017753
_cod_database_fobs_code          2017753