Tris[bis(diethylenetriamine)nickel(II)] bis[hexacyanoferrate(III)] decahydrate
Muga, Iñaki; Vitoria, Pablo; Gutiérrez-Zorrilla, Juan M.; Luque, Antonio; Román, Pascual; Acta Crystallographica Section E 58 (2002) m524–m526; doi:10.1107/S160053680201591X

data_2201383
_publ_section_title
;
 Tris[bis(diethylenetriamine)nickel(II)] bis[hexacyanoferrate(III)]
 decahydrate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m524
_journal_page_last               m526
_journal_paper_doi               10.1107/S160053680201591X
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac
'[Ni (C4 H13 N3 )2 ]3 [Fe (C N )6 ]2 , 10H2 O'
_chemical_formula_moiety         'C36 H98 Fe2 N30 Ni3 O10'
_chemical_formula_sum            'C36 H98 Fe2 N30 Ni3 O10'
_chemical_formula_weight         1399.27
_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'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 104.510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.195(3)
_cell_length_b                   12.6020(10)
_cell_length_c                   19.747(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.18
_cell_measurement_theta_min      11.55
_cell_volume                     6551.7(11)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 1997); PLATON (Spek, 1990)
;
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF99 (Beurskens et al., 1999)'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9775
_diffrn_reflns_theta_full        29.98
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        4
_diffrn_standards_interval_count 90
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.348
_exptl_absorpt_correction_T_max  0.704
_exptl_absorpt_correction_T_min  0.520
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_meas      1.42
_exptl_crystal_density_method    flotation
_exptl_crystal_description       prism
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.569
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         9512
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.1005P)^2^+3.0322P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1534
_refine_ls_wR_factor_ref         0.1775
_reflns_number_gt                6070
_reflns_number_total             9512
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci6144.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2201383
_cod_database_fobs_code          2201383