Ethylenediammonium sodium tetrakis[bis(ethylenediamine-κ^2^<i>N</i>,<i>N</i>')(oxalato-κ^2^<i>O</i>^1^,<i>O</i>^2^)cobalt(III)] [pentahydrogen di(phosphatooctadecatungstate)] tetradecahydrate
Zhang, Shuzhuo; Wang, Jing; Xu, Yun; Acta Crystallographica Section E 69 (2013) m605–m606; doi:10.1107/S160053681302583X

data_2238791
_publ_section_title
;
 Ethylenediammonium sodium
 tetrakis[bis(ethylenediamine-\k^2^<i>N</i>,<i>N</i>')(oxalato-\k^2^<i>O</i>^1^,<i>O</i>^2^)cobalt(III)]
 [pentahydrogen di(phosphatooctadecatungstate)] tetradecahydrate
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m605
_journal_page_last               m606
_journal_paper_doi               10.1107/S160053681302583X
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac
'Na (C2 H10 N2) [Co (C2 O4) (C2 H8 N2)2]4, [H5 (P2 W18 O62)2], 14H2 O'
_chemical_formula_moiety
'Na +, C2 H10 N2 2+, 4(C6 H16 Co N4 O4 +), H5 O124 P4 W36 7-, 14(H2 O)'
_chemical_formula_sum            'C26 H102 Co4 N18 Na O154 P4 W36'
_chemical_formula_weight         10132.09
_chemical_name_systematic
;Ethylenediammonium sodium
tetrakis[bis(ethylenediamine-\k^2^<i>N</i>,<i>N</i>')(oxalato-\k^2^<i>O</i>^1^,<i>O</i>^2^)cobalt(III)] [pentahydrogen
di(phosphatooctadecatungsten)] tetradecahydrate
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.693(2)
_cell_angle_beta                 84.586(2)
_cell_angle_gamma                87.992(2)
_cell_formula_units_Z            1
_cell_length_a                   14.5999(4)
_cell_length_b                   16.5714(4)
_cell_length_c                   18.0165(4)
_cell_measurement_reflns_used    12336
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.50
_cell_measurement_theta_min      2.7814
_cell_volume                     4311.88(19)
_computing_cell_refinement
;
CrysAlis CCD (Oxford Diffraction, 2009)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2009)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2009)
;
_computing_molecular_graphics
'SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega 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  0.0567
_diffrn_reflns_av_sigmaI/netI    0.0766
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            49498
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.79
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    24.424
_exptl_absorpt_correction_T_max  0.3748
_exptl_absorpt_correction_T_min  0.1576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2009)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    3.904
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4464
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
?
;
_refine_diff_density_max         2.010
_refine_diff_density_min         -1.983
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1096
_refine_ls_number_reflns         17862
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0182P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0747
_reflns_number_gt                12523
_reflns_number_total             17862
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            su2626.cif
_cod_data_source_block           1
_cod_original_cell_volume        4311.88(18)
_cod_database_code               2238791