Tetracaesium Bis(diethylenetriamine-<i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>''-pentacetato)didysprosate(III) Tridecahydrate
Sakagami, Narumi; Homma, Jun-ichi; Konno, Takumi; Okamoto, Ken-ichi; Acta Crystallographica Section C 53 (1997) 1378–1381; doi:10.1107/S0108270197006021

data_2006574
_publ_contact_author
;
Dr. Narumi Sakagami
Department of Chemistry
University of Tsukuba
Tsukuba
Ibaraki 305
Japan
;
_publ_section_title
;Tetracaesium
 Bis(diethylenetriamine-<i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>''-pentacetato)didysprosate(III)
 Tridecahydrate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1378
_journal_page_last               1381
_journal_paper_doi               10.1107/S0108270197006021
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          'Cs4 [Dy2 (C14 H18 N3 O10)2] , 13H2 O'
_chemical_formula_moiety         'C28 H36 Cs4 Dy2 N6 O20, 13(H2 O)'
_chemical_formula_sum            'C28 H62 Cs4 Dy2 N6 O33'
_chemical_formula_weight         1867.44
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 96.37(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.010(10)
_cell_length_b                   9.573(3)
_cell_length_c                   25.895(4)
_cell_measurement_reflns_used    21
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.8
_cell_volume                     5422(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;MSC/AFC Diffractometer Control Software (Molecular Structure Corporation,
 1992)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1995)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  TEXSAN
_computing_structure_refinement  'DIRDIF94 (Beurskens et al., 1994)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC7S'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_sigmaI/netI    0.043
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            6795
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        -0.52
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.482
_exptl_absorpt_correction_T_max  0.254
_exptl_absorpt_correction_T_min  0.181
_exptl_absorpt_correction_type   '\y scans (North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.287
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'short needle'
_exptl_crystal_F_000             3552.00
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         '2.06 adjacent to Dy and Cs atoms'
_refine_diff_density_min         '-1.29 adjacent to Dy and Cs atoms'
_refine_ls_extinction_coef       0.00085(3)
_refine_ls_extinction_method
'Zachariasen (1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_obs   1.262
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     331
_refine_ls_number_reflns         5390
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          .0329
_refine_ls_shift/esd_max         0.0020
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00250|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         .0372
_reflns_number_observed          5390
_reflns_number_total             6620
_reflns_observed_criterion       >3.0sigma(I)
_cod_data_source_file            fg1240.cif
_cod_data_source_block           Dy-dtpa
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00250|Fo|^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1/[\s^2^(Fo) + 0.00250|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5423(2)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C28 H62 Cs4 Dy2 N6 O33 '
_cod_database_code               2006574