Bimetallic assemblies, [Ni(en)~2~]~3~[<i>M</i>(CN)~6~]~2~·3H~2~O (en = H~2~NCH~2~CH~2~NH~2~; <i>M</i> = Fe, Co)
Jakob Østerberg Eriksen; Alan Hazell; Astrid Jensen; Josua Jepsen; Rasmus Damgaard Poulsen; Acta Crystallographica Section C 56 (2000) 551–553; doi:10.1107/S0108270100001670

data_2010928
_publ_section_title
;
 Bimetallic assemblies,
 [Ni(en)~2~]~3~[<i>M</i>(CN)~6~]~2~&#x00B7;3H~2~O (en =
 H~2~NCH~2~CH~2~NH~2~; <i>M</i> = Fe, Co)
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              551
_journal_page_last               553
_journal_paper_doi               10.1107/S0108270100001670
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac
'[{Ni(C2 H8 N2 )2 }3 {Fe (CN) 6 }2 ] , 3H2 O]'
_chemical_formula_moiety         'C24 H48 Fe2 N24 Ni3 , 3H2 O'
_chemical_formula_sum            'C24 H54 Fe2 N24 Ni3 O3'
_chemical_formula_weight         1014.72
_chemical_name_systematic        ?
_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_type_scat_source           IntTabIV
_cell_angle_alpha                107.604(3)
_cell_angle_beta                 101.474(2)
_cell_angle_gamma                106.528(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6424(9)
_cell_length_b                   14.861(2)
_cell_length_c                   17.021(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.4
_cell_measurement_theta_min      2.3
_cell_volume                     2117.6(4)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
;
      ORTEPIII (Burnett & Johnson, 1996) and KRYSTAL
;
_computing_publication_material  KRYSTAL
_computing_structure_refinement  'modified ORFLS (1962) and KRYSTAL'
_computing_structure_solution
;
     SIR97 (Cascarano et al., 1996) and KRYSTAL (Hazell, 1995)'
;
_diffrn_ambient_temperature      120
_diffrn_measurement_device       'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation scans with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'x-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .017
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19479
_diffrn_reflns_reduction_process 19479
_diffrn_reflns_theta_max         29.0
_diffrn_reflns_theta_min         2.3
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.037
_exptl_absorpt_correction_T_max  .650
_exptl_absorpt_correction_T_min  .505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1052.0
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .20
_refine_diff_density_max         .52(7)
_refine_diff_density_min         -.37(7)
_refine_ls_extinction_coef       19(4)
_refine_ls_extinction_method
;
B-C type 1 Lorentzian isotropic
Becker and Coppens (1974)
;
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     509
_refine_ls_number_reflns         7456
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           .024
_refine_ls_shift/su_max          .0015
_refine_ls_shift/su_mean         .0001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .033
_reflns_number_gt                7683
_reflns_number_total             10994
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            os1101.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_site_thermal_displace_type' tag value 'Uij' was replaced with
'Uani' value 57 times.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '
1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^' was changed to 'calc'. New
tag '_refine_ls_weighting_details' was created. The value of the new
tag was set to 'w = 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2010928