Dihydronium bis(2,6-diaminopyridinium) tris(pyridine-2,6-dicarboxylato-κ^3^<i>O</i>,<i>O</i>',<i>N</i>)dysprosate(III) dihydrate
Rafizadeh, M.; Amani, V.; Acta Crystallographica Section E 62 (2006) m90–m91; doi:10.1107/S160053680504064X

data_2207940
_publ_section_title
;Dihydronium bis(2,6-diaminopyridinium)
 tris(pyridine-2,6-dicarboxylato-\k^3^<i>O</i>,<i>O</i>',<i>N</i>)dysprosate(III)
 dihydrate
;
_journal_coeditor_code           XU6059
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m90
_journal_page_last               m91
_journal_paper_doi               10.1107/S160053680504064X
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac
'(H5 O2) (C5 H8 N3)2 [Dy (C7 H3 N O4)3], 2H2 O'
_chemical_formula_moiety
'H5 O2 +, 2C5 H8 N3 +, C21 H9 Dy1 N3 O12 3-, 2H2 O'
_chemical_formula_sum            'C31 H34 Dy N9 O16'
_chemical_formula_weight         951.17
_chemical_name_systematic
;
Dihydronium bis(2,6-diaminopyridinium)
tris(pyridine-2,6-dicarboxylato-\k^3^O,O',N)dysprosate(III) dihydrate
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.483(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.654(2)
_cell_length_b                   10.579(2)
_cell_length_c                   17.972(4)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    145(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     1829.9(7)
_computing_cell_refinement       'SAINT-Plus (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1998)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      145(2)
_diffrn_measured_fraction_theta_full 0.97
_diffrn_measured_fraction_theta_max 0.97
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.095
_diffrn_reflns_av_sigmaI/netI    0.062
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18268
_diffrn_reflns_theta_full        28.5
_diffrn_reflns_theta_max         28.5
_diffrn_reflns_theta_min         2.2
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.128
_exptl_absorpt_correction_T_max  0.653
_exptl_absorpt_correction_T_min  0.406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             954
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.75
_refine_diff_density_min         -1.14
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4508
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.050
_refine_ls_R_factor_gt           0.041
_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^)+(0.053P)^2^+1.585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.097
_refine_ls_wR_factor_ref         0.101
_reflns_number_gt                3876
_reflns_number_total             4508
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            xu6059.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1830.0(7)
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               2207940
_cod_database_fobs_code          2207940