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_2016201
_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
'[Nd (C12 H24 O6) (H2 O)4] [Fe (C N)6], 2H2 O'
_chemical_formula_moiety         'C12 H32 Nd O10 3+, C6 Fe N6 3-, 2(H2 O)'
_chemical_formula_sum            'C18 H36 Fe N6 Nd O12'
_chemical_formula_weight         728.62
_chemical_name_systematic
;
Tetraaqua(18-crown-6)neodymium(III) hexacyanoferrate(III) dihydrate
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 113.4189(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.9552(6)
_cell_length_b                   11.5063(2)
_cell_length_c                   13.9706(3)
_cell_measurement_reflns_used    3360
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.42
_cell_volume                     2943.55(12)
_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 0.997
_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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21701
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.42
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.300
_exptl_absorpt_correction_T_max  0.561
_exptl_absorpt_correction_T_min  0.478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.825
_refine_diff_density_min         -1.073
_refine_ls_extinction_coef       0.00110(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         3360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.0184
_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^)+(0.0166P)^2^+4.6543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0425
_refine_ls_wR_factor_ref         0.0433
_reflns_number_gt                3168
_reflns_number_total             3360
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gg3119.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2016201
_cod_database_fobs_code          2016201