Cyano-Bridged Bimetallic Assemblies from Hexacyanometalate, [M(CN)6]3- (M = MnIII and FeIII), and [M(N4-macrocycle)]2+ (M = FeIII, NiII and ZnII) Building Blocks. Syntheses, Multidimensional Structures, and Magnetic Properties
Enrique Colacio; Mustapha Ghazi; Helen Stoeckli-Evans; Francesc Lloret; José María Moreno; Cristina Pérez; Inorganic Chemistry 40 (2001) 4876–4883; doi:10.1021/ic0103446

data_4320248
_publ_contact_author
;
J.M. Moreno
Departamento de Qu\'imica Inorg\'anica.
Facultad de Ciencias.
Universidad de Granada
18071-Granada
SPAIN
;
_publ_contact_author_email       jmoreno@ugr.es
_publ_contact_author_fax         34-958-243322
_publ_contact_author_phone       34-958-243236
_publ_section_title
;
 Cyano-Bridged Bimetallic Assemblies from Hexacyanometalate, [M(CN)6]3- (M
 = MnIII and FeIII), and [M(N4-macrocycle)]2+ (M = FeIII, NiII and ZnII)
 Building Blocks. Syntheses, Multidimensional Structures, and Magnetic
 Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4876
_journal_page_last               4883
_journal_paper_doi               10.1021/ic0103446
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C22 H61 Fe N12 O11.5 Zn1.5'
_chemical_formula_weight         831.73
_chemical_name_systematic
;

?

;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-A 2yab'
_symmetry_space_group_name_H-M   'A 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.938(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.5474(11)
_cell_length_b                   37.056(2)
_cell_length_c                   14.7173(13)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.93
_cell_measurement_theta_min      2.11
_cell_volume                     7914.9(10)
_computing_cell_refinement       'CELL (Stoe & Cie GmbH, Darmstadt, 1997)'
_computing_data_collection       'EXPOSE (Stoe & Cie GmbH, Darmstadt, 1997)'
_computing_data_reduction
'INTEGRATE (Stoe & Cie GmbH, Darmstadt, 1997)'
_computing_molecular_graphics    'PLATON/PLUTON (Spek, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 0.81\%A
_diffrn_measured_fraction_theta_full 0.462
_diffrn_measured_fraction_theta_max 0.462
_diffrn_measurement_device_type  'STOE Image Plate Diffraction System'
_diffrn_measurement_method       'phi rotation 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  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31101
_diffrn_reflns_theta_full        25.93
_diffrn_reflns_theta_max         25.93
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    1.332
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3520
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.819
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       0.00002(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.804
_refine_ls_hydrogen_treatment    'riding atoms'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         7251
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.804
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0752P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1187
_reflns_number_gt                3724
_reflns_number_total             7251
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0103446_1.cif
_cod_data_source_block           complex5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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 'calc
w=1/[\s^2^(Fo^2^)+(0.0752P)^2^] where P=(Fo^2^+2Fc^2^)/3' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0752P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7914.8(11)
_cod_original_sg_symbol_H-M      'A 2/n'
_cod_original_formula_sum        'C22 H61 Fe N12 O11.50 Zn1.50'
_cod_database_code               4320248