#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/86/2218636.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2218636
loop_
_publ_author_name
'Zhang, Xiutang'
'Wei, Peihai'
'Li, Bin'
_publ_section_title
Diaqua-1κO,3κO-di-μ-cyanido-1:2κ²N:C;2:3κ²C:N-dicyanido-2κ²C-bis{4,4'-dibromo-2,2'-[propane-1,2-diylbis(nitrilomethylidyne)]diphenolato}-1κ⁴O,N,N',O';3κ⁴O,N,N',O'-1,3-diiron(III)-2-nickel(II)
_journal_coeditor_code           CF2205
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m926
_journal_paper_doi               10.1107/S1600536808017893
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac
'[Fe2 Ni (C17 H14 Br2 N2 O2)2 (C N)4 (H2 O)2]'
_chemical_formula_moiety         'C38 H32 Br4 Fe2 N8 Ni O6'
_chemical_formula_sum            'C38 H32 Br4 Fe2 N8 Ni O6'
_chemical_formula_weight         1186.71
_chemical_name_systematic
;Diaqua-1κO,3κO-di-μ-cyanido-
1:2κ²N:C;2:3κ²C:N-dicyanido-2κ²C-
bis{4,4'-dibromo-2,2'-[propane-1,2-diylbis(nitrilomethylidyne)]diphenolato}-
1κ⁴O,N,N',O';3κ⁴O,N,N',
O'-1,3-diiron(III)-2-nickel(II)
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.04(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.599(2)
_cell_length_b                   13.538(3)
_cell_length_c                   14.715(3)
_cell_measurement_reflns_used    3699
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      3.01
_cell_volume                     2141.8(9)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω'
_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  0.0847
_diffrn_reflns_av_sigmaI/netI    0.0909
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13404
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.889
_exptl_absorpt_correction_T_max  0.641
_exptl_absorpt_correction_T_min  0.449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.840
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.637
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         3699
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1131
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.09P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1511
_refine_ls_wR_factor_ref         0.1806
_reflns_number_gt                2263
_reflns_number_total             3699
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cf2205.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2141.8(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2218636
_cod_database_fobs_code          2218636
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Fe Fe1 0.29547(11) 0.95323(8) 0.36728(8) 0.0341(4) Uani d . 1
Ni Ni1 0.0000 1.0000 0.0000 0.0334(4) Uani d S 1
Br Br1 -0.07330(10) 1.37221(7) 0.43825(7) 0.0569(4) Uani d . 1
Br Br2 0.75936(10) 0.61244(8) 0.30711(8) 0.0621(4) Uani d . 1
C C1 0.1210(8) 0.9936(5) 0.1261(6) 0.035(2) Uani d . 1
C C2 -0.0637(8) 0.8804(6) 0.0276(6) 0.037(2) Uani d . 1
C C3 0.2234(8) 1.1459(6) 0.4134(6) 0.034(2) Uani d . 1
C C4 0.2476(8) 1.2492(5) 0.4247(5) 0.033(2) Uani d . 1
H H4 0.3242 1.2728 0.4277 0.039 Uiso calc R 1
C C5 0.1608(9) 1.3146(6) 0.4311(6) 0.042(2) Uani d . 1
H H5 0.1780 1.3819 0.4362 0.050 Uiso calc R 1
C C6 0.0471(9) 1.2807(6) 0.4303(6) 0.042(2) Uani d . 1
C C7 0.0185(9) 1.1818(6) 0.4197(6) 0.045(2) Uani d . 1
H H7 -0.0581 1.1603 0.4187 0.054 Uiso calc R 1
C C8 0.1029(8) 1.1136(5) 0.4104(6) 0.037(2) Uani d . 1
C C9 0.0680(8) 1.0105(6) 0.3966(6) 0.035(2) Uani d . 1
H H9 -0.0079 0.9939 0.4004 0.042 Uiso calc R 1
C C10 0.0874(10) 0.8350(7) 0.3700(9) 0.067(3) Uani d . 1
H H10A 0.1154 0.8044 0.4343 0.080 Uiso calc R 1
H H10B -0.0028 0.8331 0.3424 0.080 Uiso calc R 1
C C11 0.1355(9) 0.7815(7) 0.3082(9) 0.067(3) Uani d . 1
H H11 0.0893 0.8088 0.2429 0.080 Uiso calc R 1
C C12 0.1048(10) 0.6739(6) 0.2961(8) 0.060(3) Uani d . 1
H H12A 0.1567 0.6390 0.3537 0.091 Uiso calc R 1
H H12B 0.1188 0.6491 0.2400 0.091 Uiso calc R 1
H H12C 0.0191 0.6646 0.2869 0.091 Uiso calc R 1
C C13 0.3443(8) 0.7546(5) 0.3198(5) 0.032(2) Uani d . 1
H H13 0.3196 0.6893 0.3047 0.039 Uiso calc R 1
C C14 0.4688(8) 0.7786(6) 0.3302(5) 0.033(2) Uani d . 1
C C15 0.5437(9) 0.7030(6) 0.3193(5) 0.038(2) Uani d . 1
H H15 0.5141 0.6384 0.3116 0.046 Uiso calc R 1
C C16 0.6591(9) 0.7209(7) 0.3197(6) 0.049(3) Uani d . 1
C C17 0.7053(9) 0.8158(7) 0.3289(6) 0.048(2) Uani d . 1
H H17 0.7829 0.8280 0.3262 0.058 Uiso calc R 1
C C18 0.6337(8) 0.8932(6) 0.3422(6) 0.039(2) Uani d . 1
H H18 0.6657 0.9570 0.3509 0.047 Uiso calc R 1
C C19 0.5155(8) 0.8770(6) 0.3428(5) 0.033(2) Uani d . 1
N N1 0.1906(7) 0.9903(4) 0.2063(5) 0.0368(18) Uani d . 1
N N2 -0.0938(7) 0.8039(5) 0.0441(5) 0.046(2) Uani d . 1
N N3 0.1306(6) 0.9396(5) 0.3796(5) 0.0400(18) Uani d . 1
N N4 0.2649(6) 0.8131(4) 0.3289(4) 0.0294(16) Uani d . 1
O O1 0.4524(5) 0.9530(3) 0.3561(4) 0.0309(13) Uani d . 1
O O2 0.3095(5) 1.0870(4) 0.4047(4) 0.0308(13) Uani d . 1
O O3 0.3783(5) 0.9024(4) 0.5250(4) 0.0352(14) Uani d D 1
H H1W 0.433(5) 0.942(3) 0.547(6) 0.042 Uiso d D 1
H H2W 0.397(6) 0.8444(16) 0.530(6) 0.042 Uiso d D 1
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'
N N 0.0061 0.0033 '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'
Ni Ni 0.3393 1.1124 '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'
Br Br -0.2901 2.4595 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O2 Fe1 O1 . . 92.7(2)
O2 Fe1 N4 . . 174.5(3)
O1 Fe1 N4 . . 92.8(3)
O2 Fe1 N3 . . 92.5(2)
O1 Fe1 N3 . . 174.6(2)
N4 Fe1 N3 . . 82.0(3)
O2 Fe1 O3 . . 92.1(2)
O1 Fe1 O3 . . 92.1(2)
N4 Fe1 O3 . . 87.8(2)
N3 Fe1 O3 . . 86.1(3)
O2 Fe1 N1 . . 92.7(2)
O1 Fe1 N1 . . 93.8(2)
N4 Fe1 N1 . . 86.9(2)
N3 Fe1 N1 . . 87.6(3)
O3 Fe1 N1 . . 172.3(2)
C1 Ni1 C1 3_575 . 180.0(4)
C1 Ni1 C2 3_575 . 92.6(3)
C1 Ni1 C2 . . 87.4(3)
C1 Ni1 C2 3_575 3_575 87.4(3)
C1 Ni1 C2 . 3_575 92.6(3)
C2 Ni1 C2 . 3_575 180.0000(10)
N1 C1 Ni1 . . 176.0(9)
N2 C2 Ni1 . . 174.3(8)
O2 C3 C4 . . 118.7(8)
O2 C3 C8 . . 124.7(7)
C4 C3 C8 . . 116.5(7)
C5 C4 C3 . . 121.7(8)
C5 C4 H4 . . 119.2
C3 C4 H4 . . 119.2
C4 C5 C6 . . 120.3(8)
C4 C5 H5 . . 119.9
C6 C5 H5 . . 119.9
C7 C6 C5 . . 120.6(8)
C7 C6 Br1 . . 119.4(7)
C5 C6 Br1 . . 119.9(6)
C6 C7 C8 . . 120.7(9)
C6 C7 H7 . . 119.7
C8 C7 H7 . . 119.7
C7 C8 C9 . . 119.0(9)
C7 C8 C3 . . 120.2(8)
C9 C8 C3 . . 120.8(7)
N3 C9 C8 . . 126.9(8)
N3 C9 H9 . . 116.6
C8 C9 H9 . . 116.6
C11 C10 N3 . . 110.1(8)
C11 C10 H10A . . 109.6
N3 C10 H10A . . 109.6
C11 C10 H10B . . 109.6
N3 C10 H10B . . 109.6
H10A C10 H10B . . 108.2
C10 C11 N4 . . 109.3(8)
C10 C11 C12 . . 115.9(10)
N4 C11 C12 . . 119.0(8)
C10 C11 H11 . . 103.5
N4 C11 H11 . . 103.5
C12 C11 H11 . . 103.5
C11 C12 H12A . . 109.5
C11 C12 H12B . . 109.5
H12A C12 H12B . . 109.5
C11 C12 H12C . . 109.5
H12A C12 H12C . . 109.5
H12B C12 H12C . . 109.5
N4 C13 C14 . . 126.5(7)
N4 C13 H13 . . 116.8
C14 C13 H13 . . 116.8
C15 C14 C19 . . 118.8(8)
C15 C14 C13 . . 118.0(7)
C19 C14 C13 . . 123.0(7)
C16 C15 C14 . . 121.7(8)
C16 C15 H15 . . 119.2
C14 C15 H15 . . 119.2
C15 C16 C17 . . 120.9(9)
C15 C16 Br2 . . 119.5(7)
C17 C16 Br2 . . 119.6(8)
C16 C17 C18 . . 118.9(9)
C16 C17 H17 . . 120.5
C18 C17 H17 . . 120.5
C19 C18 C17 . . 121.5(8)
C19 C18 H18 . . 119.2
C17 C18 H18 . . 119.2
O1 C19 C18 . . 118.8(8)
O1 C19 C14 . . 123.0(8)
C18 C19 C14 . . 118.2(8)
C1 N1 Fe1 . . 165.6(7)
C9 N3 C10 . . 122.3(8)
C9 N3 Fe1 . . 125.4(6)
C10 N3 Fe1 . . 112.3(6)
C13 N4 C11 . . 121.5(7)
C13 N4 Fe1 . . 125.1(6)
C11 N4 Fe1 . . 113.4(5)
C19 O1 Fe1 . . 128.4(5)
C3 O2 Fe1 . . 128.5(5)
Fe1 O3 H1W . . 100(6)
Fe1 O3 H2W . . 112(6)
H1W O3 H2W . . 118(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Fe1 O2 . 1.882(5)
Fe1 O1 . 1.888(6)
Fe1 N4 . 1.973(6)
Fe1 N3 . 1.996(7)
Fe1 O3 . 2.261(5)
Fe1 N1 . 2.276(6)
Ni1 C1 3_575 1.862(8)
Ni1 C1 . 1.862(8)
Ni1 C2 . 1.886(9)
Ni1 C2 3_575 1.886(9)
Br1 C6 . 1.903(9)
Br2 C16 . 1.924(9)
C1 N1 . 1.154(10)
C2 N2 . 1.148(9)
C3 O2 . 1.322(9)
C3 C4 . 1.423(10)
C3 C8 . 1.449(12)
C4 C5 . 1.371(11)
C4 H4 . 0.930
C5 C6 . 1.393(13)
C5 H5 . 0.930
C6 C7 . 1.374(11)
C7 C8 . 1.389(12)
C7 H7 . 0.930
C8 C9 . 1.445(10)
C9 N3 . 1.284(10)
C9 H9 . 0.930
C10 C11 . 1.430(13)
C10 N3 . 1.490(11)
C10 H10A . 0.970
C10 H10B . 0.970
C11 N4 . 1.478(11)
C11 C12 . 1.494(11)
C11 H11 . 0.980
C12 H12A . 0.960
C12 H12B . 0.960
C12 H12C . 0.960
C13 N4 . 1.260(9)
C13 C14 . 1.431(11)
C13 H13 . 0.930
C14 C15 . 1.390(11)
C14 C19 . 1.424(11)
C15 C16 . 1.359(13)
C15 H15 . 0.930
C16 C17 . 1.378(12)
C17 C18 . 1.396(12)
C17 H17 . 0.930
C18 C19 . 1.392(12)
C18 H18 . 0.930
C19 O1 . 1.318(9)
O3 H1W . 0.80(6)
O3 H2W . 0.81(2)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O3 H1W O1 3_676 0.81(2) 2.09(4) 2.859(7) 159(8)
O3 H2W N2 4_676 0.81(2) 2.02(2) 2.813(9) 167(7)
