#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:30:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179331 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/28/4322882.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_4322882
loop_
_publ_author_name
'Zhiqiang Xu'
'Laurence K. Thompson'
'David O. Miller'
'Howard J. Clase'
'Judith A. K. Howard'
'Andrés E. Goeta'
_publ_section_title
;
 Spiral Dinuclear Complexes of Tetradentate N4 Diazine Ligands with
 Mn(II), Fe(II), Fe(III), Co(III), and Ni(II) Salts
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3620
_journal_page_last               3627
_journal_paper_doi               10.1021/ic9715761
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety         '[Fe2 (C10 H10 N8)3]4+, 4(N O3), 5(H2 O)'
_chemical_formula_sum            'C60 H80 Fe4 N56 O34'
_chemical_formula_weight         2353.20
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 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                 96.852(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   14.039(3)
_cell_length_b                   11.335(6)
_cell_length_c                   14.6517(15)
_cell_measurement_reflns_used    13
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      33.42
_cell_measurement_theta_min      27.64
_cell_volume                     2314.9(13)
_computing_cell_refinement       'Texray (MSC 1985)'
_computing_data_collection       'Texray (MSC 1985)'
_computing_data_reduction        'Texray (MSC 1985)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      299(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku AFC6S 4 circle'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4102
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.61
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.730
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'thick plate'
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         4102
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0600P)²+2.1411P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1260
_reflns_number_gt                3153
_reflns_number_total             4102
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9715761_4.cif
_cod_data_source_block           x554a(5)
_cod_depositor_comments
;
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 'calc
w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+2.1411P] 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^)+(0.0600P)^2^+2.1411P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               4322882
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y, z+1/2'
'-x, -y, -z'
'-x-1/2, y, -z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.36406(3) 0.76527(4) 0.20767(3) 0.02488(16) Uani 1 d . . .
C1 C 0.5196(3) 0.5939(4) 0.1836(3) 0.0458(10) Uani 1 d . . .
H1 H 0.5638 0.6483 0.2106 0.055 Uiso 1 calc R . .
C2 C 0.5517(3) 0.4885(5) 0.1506(4) 0.0682(14) Uani 1 d . . .
H2 H 0.6175 0.4749 0.1559 0.082 Uiso 1 calc R . .
C4 C 0.4002(3) 0.4283(4) 0.1095(4) 0.0633(13) Uani 1 d . . .
H4 H 0.3567 0.3708 0.0862 0.076 Uiso 1 calc R . .
C5 C 0.3657(3) 0.5333(3) 0.1401(3) 0.0382(8) Uani 1 d . . .
C6 C 0.2634(3) 0.5652(3) 0.1364(2) 0.0335(8) Uani 1 d . . .
N1 N 0.4257(2) 0.6185(2) 0.17725(19) 0.0313(6) Uani 1 d . . .
N2 N 0.25237(19) 0.6761(2) 0.15561(18) 0.0266(6) Uani 1 d . . .
N3 N 0.1927(3) 0.4870(3) 0.1192(3) 0.0536(10) Uani 1 d . . .
H3A H 0.129(3) 0.514(4) 0.116(3) 0.064 Uiso 1 d . . .
H3B H 0.201(3) 0.422(5) 0.115(3) 0.064 Uiso 1 d . . .
N4 N 0.4935(3) 0.4062(4) 0.1119(3) 0.0782(14) Uani 1 d . . .
C11 C 0.5497(3) 0.8947(3) 0.2520(3) 0.0405(9) Uani 1 d . . .
H11 H 0.5544 0.9012 0.1894 0.049 Uiso 1 calc R . .
C12 C 0.6193(3) 0.9458(4) 0.3147(3) 0.0509(11) Uani 1 d . . .
H12 H 0.6696 0.9851 0.2920 0.061 Uiso 1 calc R . .
C14 C 0.5458(3) 0.8819(4) 0.4329(3) 0.0442(9) Uani 1 d . . .
H14 H 0.5423 0.8761 0.4958 0.053 Uiso 1 calc R . .
C15 C 0.4757(2) 0.8281(3) 0.3732(2) 0.0300(7) Uani 1 d . . .
C16 C 0.3927(2) 0.7629(3) 0.4011(2) 0.0309(7) Uani 1 d . . .
N11 N 0.47562(19) 0.8362(2) 0.28045(19) 0.0291(6) Uani 1 d . . .
N12 N 0.33996(19) 0.7166(2) 0.33057(17) 0.0260(6) Uani 1 d . . .
N13 N 0.3750(3) 0.7586(4) 0.4873(2) 0.0535(10) Uani 1 d . . .
H13A H 0.327(3) 0.724(4) 0.508(3) 0.064 Uiso 1 d . . .
H13B H 0.411(3) 0.790(4) 0.529(3) 0.064 Uiso 1 d . . .
N14 N 0.6187(2) 0.9422(3) 0.4043(2) 0.0534(9) Uani 1 d . . .
C21 C 0.4301(3) 0.8065(3) 0.0243(2) 0.0377(8) Uani 1 d . . .
H21 H 0.4625 0.7349 0.0309 0.045 Uiso 1 calc R . .
C22 C 0.4335(3) 0.8712(4) -0.0548(3) 0.0458(10) Uani 1 d . . .
H22 H 0.4671 0.8408 -0.1004 0.055 Uiso 1 calc R . .
C24 C 0.3422(3) 1.0135(4) -0.0008(2) 0.0393(9) Uani 1 d . . .
H24 H 0.3120 1.0865 -0.0073 0.047 Uiso 1 calc R . .
C25 C 0.3351(2) 0.9492(3) 0.0780(2) 0.0267(7) Uani 1 d . . .
C26 C 0.2744(2) 0.9806(3) 0.1499(2) 0.0256(7) Uani 1 d . . .
N21 N 0.38128(19) 0.8439(2) 0.09211(18) 0.0284(6) Uani 1 d . . .
N22 N 0.28406(18) 0.9056(2) 0.21797(17) 0.0242(6) Uani 1 d . . .
N23 N 0.2139(2) 1.0702(3) 0.1391(2) 0.0383(8) Uani 1 d . . .
H23A H 0.173(3) 1.088(4) 0.180(3) 0.046 Uiso 1 d . . .
H23B H 0.210(3) 1.115(4) 0.101(3) 0.046 Uiso 1 d . . .
N24 N 0.3908(3) 0.9753(3) -0.0685(2) 0.0486(9) Uani 1 d . . .
N10 N 0.0148(3) 0.2005(4) 0.2083(3) 0.0622(11) Uani 1 d . . .
O11 O -0.0690(4) 0.2239(6) 0.2212(4) 0.138(2) Uani 1 d . . .
O12 O 0.0406(4) 0.2284(5) 0.1363(3) 0.123(2) Uani 1 d . . .
O13 O 0.0673(3) 0.1443(4) 0.2648(2) 0.0815(12) Uani 1 d . . .
N20 N 0.7618(3) 0.6932(4) 0.0744(3) 0.0637(11) Uani 1 d . . .
O21 O 0.7829(3) 0.7214(3) -0.0039(2) 0.0673(9) Uani 1 d . . .
O22 O 0.8162(4) 0.6284(5) 0.1244(3) 0.1190(18) Uani 1 d . . .
O23 O 0.6889(3) 0.7309(4) 0.1008(4) 0.1118(17) Uani 1 d . . .
O1W O -0.0096(9) 0.4983(11) 0.1040(10) 0.080(3) Uani 0.67 d P A 1
O1WA O -0.022(2) 0.541(2) 0.082(2) 0.086(7) Uani 0.33 d P B 2
O2W O 0.2561(5) 0.6238(6) 0.5923(5) 0.173(3) Uani 1 d . . .
O3W O 0.2500 0.7489(14) 0.7500 0.267(7) Uani 1 d S . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N1 79.97(12) . . ?
N2 Fe1 N12 89.68(11) . . ?
N1 Fe1 N12 95.75(11) . . ?
N2 Fe1 N21 94.29(12) . . ?
N1 Fe1 N21 94.99(11) . . ?
N12 Fe1 N21 169.05(11) . . ?
N2 Fe1 N11 169.19(11) . . ?
N1 Fe1 N11 97.27(12) . . ?
N12 Fe1 N11 80.16(11) . . ?
N21 Fe1 N11 96.37(12) . . ?
N2 Fe1 N22 90.54(11) . . ?
N1 Fe1 N22 169.01(11) . . ?
N12 Fe1 N22 89.68(11) . . ?
N21 Fe1 N22 80.10(11) . . ?
N11 Fe1 N22 93.06(11) . . ?
N1 C1 C2 121.0(4) . . ?
N4 C2 C1 123.2(4) . . ?
N4 C4 C5 122.5(4) . . ?
N1 C5 C4 121.3(4) . . ?
N1 C5 C6 113.4(3) . . ?
C4 C5 C6 125.3(4) . . ?
N2 C6 N3 125.3(3) . . ?
N2 C6 C5 111.7(3) . . ?
N3 C6 C5 123.0(3) . . ?
C1 N1 C5 116.1(3) . . ?
C1 N1 Fe1 128.4(3) . . ?
C5 N1 Fe1 115.4(2) . . ?
C6 N2 N12 118.7(3) . 4_656 ?
C6 N2 Fe1 118.4(2) . . ?
N12 N2 Fe1 119.07(19) 4_656 . ?
C2 N4 C4 115.8(4) . . ?
N11 C11 C12 120.9(4) . . ?
N14 C12 C11 124.1(4) . . ?
N14 C14 C15 122.7(4) . . ?
N11 C15 C14 121.3(3) . . ?
N11 C15 C16 113.8(3) . . ?
C14 C15 C16 124.8(3) . . ?
N12 C16 N13 126.1(3) . . ?
N12 C16 C15 111.8(3) . . ?
N13 C16 C15 122.0(3) . . ?
C11 N11 C15 115.8(3) . . ?
C11 N11 Fe1 129.3(2) . . ?
C15 N11 Fe1 114.9(2) . . ?
C16 N12 N2 117.4(3) . 4_656 ?
C16 N12 Fe1 118.2(2) . . ?
N2 N12 Fe1 119.17(19) 4_656 . ?
C12 N14 C14 115.2(3) . . ?
N21 C21 C22 121.8(3) . . ?
N24 C22 C21 122.8(3) . . ?
N24 C24 C25 122.9(3) . . ?
N21 C25 C24 120.7(3) . . ?
N21 C25 C26 114.1(3) . . ?
C24 C25 C26 125.1(3) . . ?
N22 C26 N23 126.8(3) . . ?
N22 C26 C25 111.8(3) . . ?
N23 C26 C25 121.2(3) . . ?
C21 N21 C25 116.1(3) . . ?
C21 N21 Fe1 128.6(2) . . ?
C25 N21 Fe1 115.2(2) . . ?
C26 N22 N22 119.2(3) . 4_656 ?
C26 N22 Fe1 118.5(2) . . ?
N22 N22 Fe1 119.22(12) 4_656 . ?
C22 N24 C24 115.7(3) . . ?
O12 N10 O13 120.9(4) . . ?
O12 N10 O11 118.0(5) . . ?
O13 N10 O11 121.0(5) . . ?
O23 N20 O22 120.3(5) . . ?
O23 N20 O21 120.0(5) . . ?
O22 N20 O21 119.7(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.943(3) . ?
Fe1 N1 1.951(3) . ?
Fe1 N12 1.951(3) . ?
Fe1 N21 1.954(3) . ?
Fe1 N11 1.959(3) . ?
Fe1 N22 1.963(3) . ?
C1 N1 1.340(5) . ?
C1 C2 1.384(6) . ?
C2 N4 1.322(6) . ?
C4 N4 1.329(6) . ?
C4 C5 1.381(5) . ?
C5 N1 1.353(5) . ?
C5 C6 1.474(5) . ?
C6 N2 1.302(4) . ?
C6 N3 1.332(5) . ?
N2 N12 1.412(4) 4_656 ?
C11 N11 1.341(4) . ?
C11 C12 1.386(6) . ?
C12 N14 1.314(5) . ?
C14 N14 1.339(5) . ?
C14 C15 1.379(5) . ?
C15 N11 1.361(4) . ?
C15 C16 1.478(5) . ?
C16 N12 1.308(4) . ?
C16 N13 1.316(5) . ?
N12 N2 1.412(4) 4_656 ?
C21 N21 1.341(4) . ?
C21 C22 1.377(5) . ?
C22 N24 1.328(5) . ?
C24 N24 1.341(5) . ?
C24 C25 1.379(5) . ?
C25 N21 1.362(4) . ?
C25 C26 1.477(4) . ?
C26 N22 1.306(4) . ?
C26 N23 1.320(4) . ?
N22 N22 1.418(5) 4_656 ?
N10 O12 1.199(5) . ?
N10 O13 1.221(5) . ?
N10 O11 1.242(6) . ?
N20 O23 1.214(5) . ?
N20 O22 1.236(5) . ?
N20 O21 1.259(5) . ?
