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_2016205
_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
'[Gd (C12 H24 O6) (H2 O)3] [Co (C N)6], 2H2 O'
_chemical_formula_moiety         'C12 H30 Gd O9 3+, C6 Co N6 3-, 2(H2 O)'
_chemical_formula_sum            'C18 H34 Co Gd N6 O11'
_chemical_formula_weight         726.69
_chemical_name_systematic
;
triaqua(18-crown-6)gadolinium(III) hexacyanocobaltate(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
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_cell_angle_beta                 70.5870(8)
_cell_angle_gamma                65.5666(9)
_cell_formula_units_Z            2
_cell_length_a                   10.8604(2)
_cell_length_b                   11.0724(3)
_cell_length_c                   13.9909(2)
_cell_measurement_reflns_used    6164
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1385.20(5)
_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 0.989
_diffrn_measurement_device_type  'Bruker--Nonius KappaCCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
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_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            27907
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.57
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_diffrn_standards_decay_%        0
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_exptl_absorpt_correction_T_min  0.187
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             726
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.42
_refine_diff_density_max         0.997
_refine_diff_density_min         -0.908
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         6348
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0197
_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^)+(0.0144P)^2^+1.6153P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.0466
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_reflns_number_total             6348
_reflns_threshold_expression     I>2\s(I)
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_cod_database_code               2016205
_cod_database_fobs_code          2016205