Hydrated hexacyanometallate(III) salts of triaqua(18-crown-6)lanthanoid(III) and tetraaqua(18-crown-6)lanthanoid(III) cations containing nine- and ten-coordinate lanthanoids
Misra, Phalguni; Koner, Rajesh; Nayak, Malabika; Mohanta, Sasankasekhar; Low, John N.; Ferguson, George; Glidewell, Christopher; Acta Crystallographica Section C 63 (2007) m440–m444; doi:10.1107/S0108270107040449

data_2016202
_publ_section_title
;
 Hydrated hexacyanometallate(III) salts of
 triaqua(18-crown-6)lanthanoid(III) and
 tetraaqua(18-crown-6)lanthanoid(III) cations containing nine- and
 ten-coordinate lanthanoids
;
_journal_coeditor_code           GG3119
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m440
_journal_page_last               m444
_journal_paper_doi               10.1107/S0108270107040449
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac
'[Sm (C12 H24 O6) (H2 O)3] [Fe (C N)6], 2H2 O'
_chemical_formula_moiety         'C12 H30 O9 Sm 3+, C6 Fe N6 3-, 2(H2 O)'
_chemical_formula_sum            'C18 H34 Fe N6 O11 Sm'
_chemical_formula_weight         716.71
_chemical_name_systematic
;
Triaqua(18-crown-6)samarium(III) hexacyanoferrate(III) 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
_cell_angle_alpha                67.9012(13)
_cell_angle_beta                 70.7291(13)
_cell_angle_gamma                65.7231(14)
_cell_formula_units_Z            2
_cell_length_a                   10.9324(2)
_cell_length_b                   11.0996(2)
_cell_length_c                   14.0119(4)
_cell_measurement_reflns_used    6393
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1404.76(6)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) and COLLECT'
_computing_data_collection       'COLLECT (Hooft, 1999)'
_computing_data_reduction        'DENZO and COLLECT'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL97 and PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement  'OSCAIL and SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution
'OSCAIL (McArdle, 2003) and SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker--Nonius KappaCCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker--Nonius FR591 rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28348
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         3.42
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.647
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.945
_refine_diff_density_min         -0.910
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         6453
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+2.0082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0671
_reflns_number_gt                5624
_reflns_number_total             6453
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gg3119.cif
_cod_data_source_block           III
_cod_original_cell_volume        1404.77(6)
_cod_original_formula_sum        'C18 H34 Fe1 N6 O11 Sm'
_cod_database_code               2016202
_cod_database_fobs_code          2016202