#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/75/4317551.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4317551
loop_
_publ_author_name
'Rodrigue Lescouëzec'
'Francesc Lloret'
'Miguel Julve'
'Jacqueline Vaissermann'
'Michel Verdaguer'
_publ_contact_author_email       ' miguel.julve@uv.es '
_publ_contact_author_fax         ' 0034 398 3001 '
_publ_contact_author_phone       ' 0034 386 4856 '
_publ_section_title
;
 [Fe(bipy)(CN)4]- as a Versatile Building Block for the Design of
 Heterometallic Systems: Synthesis, Crystal Structure, and Magnetic
 Properties of PPh4[FeIII(bipy)(CN)4].H2O,
 [{FeIII(bipy)(CN)4}2MII(H2O)4].4H2O, and [{FeIII(bipy)(CN)4}2ZnII].2H2O
 [bipy = 2,2'-Bipyridine; M = Mn and Zn]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              818
_journal_page_last               826
_journal_paper_doi               10.1021/ic0107882
_journal_volume                  41
_journal_year                    2002
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C28 H24 Fe2 Zn1 N12 O4 ,4 H2O '
_chemical_formula_sum            'C28 H32 Fe2 N12 O8 Zn'
_chemical_formula_weight         841.7
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             01-02-07
_audit_creation_method           CRYSTALS
_cell_angle_alpha                90
_cell_angle_beta                 93.32(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.499(6)
_cell_length_b                   19.155(5)
_cell_length_c                   14.338(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      12
_cell_volume                     1781.9(18)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction
;
RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994)
;
_computing_molecular_graphics
;
 CAMERON (Watkin, Prout & Pearce,  1996)
;
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      295
_diffrn_measurement_device       'Enraf-nonius CAD4 '
_diffrn_measurement_method       2θ/ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.03
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3923
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1
_diffrn_standards_decay_%        4.42
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.55
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ψ scan'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.57
_exptl_crystal_description       prism
_exptl_crystal_F_000             829.73
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.60
_refine_diff_density_min         -0.36
_refine_ls_extinction_coef       35
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_obs   1.1453
_refine_ls_hydrogen_treatment
;
 H atoms placed geometrically, one overall isotropic thermal parameter refined.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         1635
_refine_ls_R_factor_obs          0.0441
_refine_ls_shift/esd_max         0.001688
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme
;
 Chebychev polynomial (Carruthers & Watkin, 1979)
;
_refine_ls_wR_factor_obs         0.0512
_reflns_number_observed          1635
_reflns_number_total             3479
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            ic0107882_3.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'EMPIRICAL'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

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

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Direct_Methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value 'Geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        1781(2)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C28 H32 Fe2 Zn1 N12 O8'
_cod_database_code               4317551
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_thermal_displace_type
FE1 0.2729(1) 0.12648(5) -0.27330(6) 0.0243 1.0000 Uani
ZN1 0.0000 0.0000 0.0000 0.0345 1.0000 Uani
O1 0.2302(9) -0.0714(3) -0.0319(3) 0.0554 1.0000 Uani
O2 -0.2485(9) -0.0652(3) -0.0581(4) 0.0567 1.0000 Uani
N1 0.0414(9) 0.0469(3) -0.1285(4) 0.0377 1.0000 Uani
N2 0.566(1) 0.1565(4) -0.1040(4) 0.0541 1.0000 Uani
N3 0.0479(9) 0.2637(3) -0.2356(4) 0.0425 1.0000 Uani
N4 0.508(1) -0.0067(3) -0.3175(5) 0.0491 1.0000 Uani
N11 0.0884(7) 0.1106(2) -0.3857(3) 0.0278 1.0000 Uani
N12 0.4288(7) 0.1791(2) -0.3650(3) 0.0238 1.0000 Uani
C1 0.121(1) 0.0762(3) -0.1849(4) 0.0317 1.0000 Uani
C2 0.4590(9) 0.1451(4) -0.1683(4) 0.0351 1.0000 Uani
C3 0.129(1) 0.2128(3) -0.2467(4) 0.0282 1.0000 Uani
C4 0.4231(9) 0.0427(4) -0.3002(4) 0.0303 1.0000 Uani
C11 -0.083(1) 0.0709(4) -0.3901(4) 0.0363 1.0000 Uani
C12 -0.199(1) 0.0636(4) -0.4734(5) 0.0402 1.0000 Uani
C13 -0.148(1) 0.0981(4) -0.5503(5) 0.0415 1.0000 Uani
C14 0.028(1) 0.1388(4) -0.5464(4) 0.0394 1.0000 Uani
C15 0.1427(9) 0.1450(3) -0.4624(4) 0.0259 1.0000 Uani
C16 0.3316(9) 0.1843(3) -0.4510(4) 0.0285 1.0000 Uani
C17 0.412(1) 0.2259(4) -0.5186(4) 0.0372 1.0000 Uani
C18 0.597(1) 0.2591(4) -0.5004(4) 0.0414 1.0000 Uani
C19 0.696(1) 0.2521(4) -0.4135(4) 0.0366 1.0000 Uani
C20 0.607(1) 0.2117(3) -0.3482(4) 0.0323 1.0000 Uani
O10 -0.2703(8) -0.1198(3) -0.2430(4) 0.0513 1.0000 Uani
O11 0.1534(9) -0.1270(3) -0.2022(4) 0.0674 1.0000 Uani
H111 -0.1255 0.0467 -0.3324 0.059(8) 1.0000 Uiso
H121 -0.3242 0.0327 -0.4759 0.059(8) 1.0000 Uiso
H131 -0.2350 0.0946 -0.6098 0.059(8) 1.0000 Uiso
H141 0.0713 0.1630 -0.6036 0.059(8) 1.0000 Uiso
H171 0.3360 0.2310 -0.5809 0.059(8) 1.0000 Uiso
H181 0.6611 0.2884 -0.5500 0.059(8) 1.0000 Uiso
H191 0.8300 0.2760 -0.3979 0.059(8) 1.0000 Uiso
H201 0.6801 0.2065 -0.2855 0.059(8) 1.0000 Uiso
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'Fe  ' 0.3010 0.8450 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805
1.0369 International_Tables_Vol_IV_Table_2.2B
'C   ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 International_Tables_Vol_IV_Table_2.2B
'Zn  ' 0.2220 1.4310 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097
1.3041 International_Tables_Vol_IV_Table_2.2B
'N   ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 International_Tables_Vol_IV_Table_2.2B
'O   ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 International_Tables_Vol_IV_Table_2.2B
'H   ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997
0.0030 International_Tables_Vol_IV_Table_2.2B
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N11 . FE1 . N12 . 81.2(2) no
N11 . FE1 . C1 . 98.6(2) no
N12 . FE1 . C1 . 179.6(2) no
N11 . FE1 . C2 . 177.1(2) no
N12 . FE1 . C2 . 95.9(2) no
C1 . FE1 . C2 . 84.3(3) no
N11 . FE1 . C3 . 90.8(2) no
N12 . FE1 . C3 . 88.2(2) no
C1 . FE1 . C3 . 91.4(3) no
C2 . FE1 . C3 . 88.7(3) no
N11 . FE1 . C4 . 89.9(2) no
N12 . FE1 . C4 . 90.4(2) no
C1 . FE1 . C4 . 90.0(3) no
C2 . FE1 . C4 . 90.4(3) no
C3 . FE1 . C4 . 178.3(3) no
O1 . ZN1 . O1 2_555 179.99 no
O1 . ZN1 . O2 . 93.7(2) no
O1 2_555 ZN1 . O2 . 86.3(2) no
O1 . ZN1 . O2 2_555 86.3(2) no
O1 2_555 ZN1 . O2 2_555 93.7(2) no
O2 . ZN1 . O2 2_555 179.99 no
O1 . ZN1 . N1 . 87.6(2) no
O1 2_555 ZN1 . N1 . 92.4(2) no
O2 . ZN1 . N1 . 92.3(2) no
O2 2_555 ZN1 . N1 . 87.7(2) no
O1 . ZN1 . N1 2_555 92.4(2) no
O1 2_555 ZN1 . N1 2_555 87.6(2) no
O2 . ZN1 . N1 2_555 87.7(2) no
O2 2_555 ZN1 . N1 2_555 92.3(2) no
N1 . ZN1 . N1 2_555 179.99 no
ZN1 . N1 . C1 . 159.0(6) no
FE1 . N11 . C11 . 125.9(4) no
FE1 . N11 . C15 . 114.5(4) no
C11 . N11 . C15 . 119.6(5) no
FE1 . N12 . C16 . 114.4(4) no
FE1 . N12 . C20 . 126.5(4) no
C16 . N12 . C20 . 119.0(5) no
FE1 . C1 . N1 . 175.5(6) no
FE1 . C2 . N2 . 178.2(6) no
FE1 . C3 . N3 . 176.6(5) no
FE1 . C4 . N4 . 178.6(6) no
N11 . C11 . C12 . 120.5(6) no
N11 . C11 . H111 . 119.4(6) no
C12 . C11 . H111 . 120.1(6) no
C11 . C12 . C13 . 120.5(6) no
C11 . C12 . H121 . 119.4(7) no
C13 . C12 . H121 . 120.1(6) no
C12 . C13 . C14 . 119.4(6) no
C12 . C13 . H131 . 120.6(7) no
C14 . C13 . H131 . 120.0(7) no
C13 . C14 . C15 . 119.1(6) no
C13 . C14 . H141 . 120.3(6) no
C15 . C14 . H141 . 120.6(6) no
N11 . C15 . C14 . 120.9(5) no
N11 . C15 . C16 . 115.2(5) no
C14 . C15 . C16 . 123.8(5) no
N12 . C16 . C15 . 114.3(5) no
N12 . C16 . C17 . 120.3(5) no
C15 . C16 . C17 . 125.3(5) no
C16 . C17 . C18 . 119.9(6) no
C16 . C17 . H171 . 119.6(6) no
C18 . C17 . H171 . 120.5(6) no
C17 . C18 . C19 . 119.0(6) no
C17 . C18 . H181 . 120.9(6) no
C19 . C18 . H181 . 120.1(7) no
C18 . C19 . C20 . 118.9(6) no
C18 . C19 . H191 . 120.8(6) no
C20 . C19 . H191 . 120.3(6) no
N12 . C20 . C19 . 122.8(6) no
N12 . C20 . H201 . 118.9(6) no
C19 . C20 . H201 . 118.4(6) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
FE1 . N11 . 1.976(5) yes
FE1 . N12 . 1.980(5) yes
FE1 . C1 . 1.913(7) yes
FE1 . C2 . 1.909(6) yes
FE1 . C3 . 1.948(7) yes
FE1 . C4 . 1.929(7) yes
ZN1 . O1 . 2.097(5) yes
ZN1 . O1 2_555 2.097(5) yes
ZN1 . O2 . 2.169(5) yes
ZN1 . O2 2_555 2.169(5) yes
ZN1 . N1 . 2.082(5) yes
ZN1 . N1 2_555 2.082(5) yes
N1 . C1 . 1.132(8) yes
N2 . C2 . 1.145(8) yes
N3 . C3 . 1.124(8) yes
N4 . C4 . 1.131(8) yes
N11 . C11 . 1.345(8) yes
N11 . C15 . 1.346(7) yes
N12 . C16 . 1.357(7) yes
N12 . C20 . 1.325(8) yes
C11 . C12 . 1.384(9) yes
C11 . H111 . 1.002(6) no
C12 . C13 . 1.34(1) yes
C12 . H121 . 1.004(7) no
C13 . C14 . 1.38(1) yes
C13 . H131 . 1.000(6) no
C14 . C15 . 1.386(8) yes
C14 . H141 . 0.997(6) no
C15 . C16 . 1.442(8) yes
C16 . C17 . 1.380(8) yes
C17 . C18 . 1.371(9) yes
C17 . H171 . 1.002(6) no
C18 . C19 . 1.374(9) yes
C18 . H181 . 1.014(6) no
C19 . C20 . 1.368(8) yes
C19 . H191 . 1.000(6) no
C20 . H201 . 0.997(6) no
