Triaquatetrakis(dimethylacetamide-κ<i>O</i>)gadolinium(III) hexacyanoferrate(III) dihydrate
Svendsen, Helle; Overgaard, Jacob; Chevalier, Marie A.; Iversen, Bo B.; Acta Crystallographica Section E 62 (2006) m989–m991; doi:10.1107/S1600536806011950

data_2208902
_publ_section_title
;
 Triaquatetrakis(dimethylacetamide-\k<i>O</i>)gadolinium(III)
 hexacyanoferrate(III) dihydrate
;
_journal_coeditor_code           HG2026
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m989
_journal_page_last               m991
_journal_paper_doi               10.1107/S1600536806011950
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac
'[Gd (C4 H9 N O)4 (H2 O)3] [Fe (C N)6], 2H2 O'
_chemical_formula_moiety         'C16 H42 Gd N4 O7 3+, C6 Fe N6 3-, 2H2 O'
_chemical_formula_sum            'C22 H46 Fe Gd N10 O9'
_chemical_formula_weight         807.77
_chemical_name_systematic
;
Triaquatetrakis(dimethylacetamide-\kO)gadolinium(III) hexacyanoferrate(III)
dihydrate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.0883(3)
_cell_length_b                   19.2620(4)
_cell_length_c                   22.2566(4)
_cell_measurement_reflns_used    8587
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.680
_cell_measurement_theta_min      4.608
_cell_volume                     6897.2(2)
_computing_cell_refinement       SAINT-Plus
_computing_data_collection       'APEX2 (Bruker--Nonius, 2004)'
_computing_data_reduction        'SAINT-Plus (Bruker--Nonius, 2004)'
_computing_molecular_graphics    'XSHELL (Bruker, 2000)'
_computing_publication_material
;
enCIFer (Version 1.1; Allen <i>et al.</i>,  2004) and WinGX (Farrugia,
1999)'
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker X8 APEX-II diffractometer'
_diffrn_measurement_method       '\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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            147578
_diffrn_reflns_reduction_process
;
 Scaled and merged with SORTAV
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        34.50
_diffrn_reflns_theta_max         35.43
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.385
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3280
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.208
_refine_diff_density_min         -0.934
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.279
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         14850
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.279
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0232P)^2^+1.8917P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0703
_reflns_number_gt                11939
_reflns_number_total             14850
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg2026.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 'Orthorhombic' changed to
'orthorhombic' 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_database_code               2208902
_cod_database_fobs_code          2208902