A holmium complex of a macrocyclic ligand (DOTA) and its isostructural europium analogue
Benetollo, Franco; Bombieri, Gabriella; Aime, Silvio; Botta, Mauro; Acta Crystallographica Section C 55 (1999) 353–356; doi:10.1107/S0108270198014450

data_2008231
_publ_section_title
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 A holmium complex of a macrocyclic ligand (DOTA) and its isostructural
 europium analogue
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              353
_journal_page_last               356
_journal_paper_doi               10.1107/S0108270198014450
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          'Na [Ho (C16 H24 N4 O8) (H2 O)], 4H2 O'
_chemical_formula_moiety         'Na [Ho (C16 H24 N4 O8) (H2 O)], 4H2 O'
_chemical_formula_sum            'C16 H34 Ho N4 Na O13'
_chemical_formula_weight         678.39
_chemical_name_systematic
;
Sodium Aquo(1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetato)holmium(III)
Tetrahydrate.
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                82.94(3)
_cell_angle_beta                 85.85(2)
_cell_angle_gamma                81.76(2)
_cell_formula_units_Z            2
_cell_length_a                   8.735(2)
_cell_length_b                   9.093(2)
_cell_length_c                   15.640(3)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      12
_cell_volume                     1218.2(5)
_computing_cell_refinement       FEBO
_computing_data_collection       'FEBO (Belletti, 1993)'
_computing_data_reduction        FEBO
_computing_molecular_graphics    'ORTEPII (Johnson 1976)'
_computing_publication_material  'PARST94 (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device_type  'Philips PW1100 four-circle'
_diffrn_measurement_method
'Profile-fitted \q/2\q scans (Lehmann & Larsen, 1974)'
_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  0.013
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5231
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  180
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.34
_exptl_absorpt_correction_T_max  0.321
_exptl_absorpt_correction_T_min  0.247
_exptl_absorpt_correction_type   '\y scan (North et al., 1968)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.34
_refine_diff_density_max         '1.758 (close to Ho)'
_refine_diff_density_min         -1.717
_refine_ls_extinction_coef       0.0077(7)
_refine_ls_extinction_method     SHELXL93
_refine_ls_goodness_of_fit_all   1.069
_refine_ls_goodness_of_fit_obs   1.069
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         5032
_refine_ls_number_restraints     'no restrains'
_refine_ls_restrained_S_all      1.092
_refine_ls_restrained_S_obs      1.069
_refine_ls_R_factor_all          0.024
_refine_ls_R_factor_obs          0.024
_refine_ls_shift/esd_max         0.009
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0486P)^2^+0.5937P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.061
_refine_ls_wR_factor_obs         0.061
_reflns_number_observed          5032
_reflns_number_total             5033
_reflns_observed_criterion       I>3\s(I)
_cod_data_source_file            cf1277.cif
_cod_data_source_block           ho
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0486P)^2^+0.5937P] where P = (Fo^2^+2Fc^2^)/3' 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^2^)+(0.0486P)^2^+0.5937P] where P = (Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               2008231