#------------------------------------------------------------------------------
#$Date: 2017-01-09 05:17:38 +0200 (Mon, 09 Jan 2017) $
#$Revision: 190118 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/10/7041023.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_7041023
loop_
_publ_author_name
'Wei, Rong-Min'
'Kong, Ming'
'Cao, Fan'
'Li, Jing'
'Pu, Tian-Cheng'
'Yang, Li'
'Zhang, Xiu-Ling'
'Song, You'
_publ_section_title
;
 Water induced spin-crossover behaviour and magneto-structural correlation
 in octacyanotungstate(iv)-based iron(ii) complexes.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18643
_journal_page_last               18652
_journal_paper_doi               10.1039/c6dt03421g
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C56 H56 Fe2 N16 O8 W'
_chemical_formula_sum            'C56 H56 Fe2 N16 O8 W'
_chemical_formula_weight         1376.71
_space_group_crystal_system      tetragonal
_space_group_IT_number           141
_space_group_name_Hall           '-I 4bd 2'
_space_group_name_H-M_alt        'I 41/a m d'
_symmetry_space_group_name_Hall  '-I 4bd 2'
_symmetry_space_group_name_H-M   'I 41/a m d :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-10-09 deposited with the CCDC.
2016-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.173(2)
_cell_length_b                   20.173(2)
_cell_length_c                   14.554(3)
_cell_measurement_reflns_used    2855
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      2.65
_cell_volume                     5922.7(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1114
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23390
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.584
_diffrn_reflns_theta_min         1.725
_exptl_absorpt_coefficient_mu    2.488
_exptl_absorpt_correction_T_max  0.689
_exptl_absorpt_correction_T_min  0.614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    not
_exptl_crystal_description       block
_exptl_crystal_F_000             2776
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.842
_refine_diff_density_min         -1.219
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         1791
_refine_ls_number_restraints     142
_refine_ls_restrained_S_all      1.265
_refine_ls_R_factor_all          0.1357
_refine_ls_R_factor_gt           0.0967
_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)+(0.1584P)²+12.3257P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2366
_refine_ls_wR_factor_ref         0.2808
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1152
_reflns_number_total             1791
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt03421g2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7041017--7041023.cif.'
_cod_original_cell_volume        5922.3(17)
_cod_database_code               7041023
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.636
_shelx_estimated_absorpt_t_max   0.707
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z+1/2'
'x, -y, -z'
'y+1/4, x+3/4, -z+1/4'
'-y+1/4, -x+1/4, -z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1'
'x+1/2, -y+1/2, -z+1/2'
'y+3/4, x+5/4, -z+3/4'
'-y+3/4, -x+3/4, -z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z-1/2'
'-x, y, z'
'-y-1/4, -x-3/4, z-1/4'
'y-1/4, x-1/4, z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'x, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'
'-y+1/4, -x-1/4, z+1/4'
'y+1/4, x+1/4, z-1/4'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
W1 W 0.5000 0.2500 0.6250 0.0691(5) Uani 1 8 d S T P
Fe1 Fe 0.5000 0.0000 0.5000 0.1080(13) Uani 1 4 d S T P
N1 N 0.5989(12) 0.2500 0.4429(12) 0.140(7) Uani 1 2 d S T P
N2 N 0.5000 0.0962(9) 0.5545(12) 0.114(5) Uani 1 2 d S T P
N4 N 0.6067(15) 0.0000 0.5000 0.178(7) Uani 1 2 d S TU P
O2 O 0.736(3) 0.1705(5) 0.392(3) 0.255(12) Uani 0.5 1 d D U P
H2A H 0.7551 0.2124 0.3559 0.382 Uiso 0.5 1 d DR U P
C1 C 0.5623(9) 0.2500 0.5050(14) 0.086(4) Uani 1 2 d S T P
C2 C 0.5000 0.1491(9) 0.5790(13) 0.091(5) Uani 1 2 d S T P
C3 C 0.6404(14) 0.0576(13) 0.493(2) 0.195(6) Uani 1 1 d . U .
H3 H 0.6177 0.0974 0.4861 0.234 Uiso 1 1 calc R U .
C4 C 0.7096(16) 0.0569(16) 0.497(3) 0.212(7) Uani 1 1 d D U .
C5 C 0.739(3) 0.0000 0.5000 0.214(9) Uani 1 2 d S TU P
H5 H 0.7848 0.0000 0.5000 0.257 Uiso 1 2 calc R U P
C6 C 0.736(3) 0.122(2) 0.463(4) 0.221(8) Uani 0.5 1 d D U P
H12A H 0.7276 0.1494 0.5158 0.266 Uiso 0.5 1 calc R U P
H12B H 0.7835 0.1127 0.4660 0.266 Uiso 0.5 1 calc R U P
N3 N 0.5000 0.044(4) 0.359(4) 0.299(12) Uani 1 2 d DS TU P
C11 C 0.5000 0.112(4) 0.350(4) 0.302(12) Uani 1 2 d DS TU P
C7 C 0.5000 0.010(3) 0.278(5) 0.306(13) Uani 1 2 d DS TU P
C9 C 0.544(3) 0.102(4) 0.200(4) 0.307(13) Uani 0.5 1 d D U P
C10 C 0.539(3) 0.141(2) 0.280(6) 0.307(12) Uani 0.5 1 d D U P
C8 C 0.5000 0.048(4) 0.198(3) 0.310(13) Uani 1 2 d DS TU P
C12 C 0.5000 0.205(3) 0.274(5) 0.312(13) Uani 1 2 d DS TU P
O1 O 0.559(2) 0.2500 0.260(3) 0.318(13) Uani 1 2 d DS TU P
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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
C2 W1 C2 143.6(10) 20_657 27_566
C2 W1 C2 95.6(3) 20_657 10_554
C2 W1 C2 95.6(3) 27_566 10_554
C2 W1 C2 95.6(3) 20_657 .
C2 W1 C2 95.6(3) 27_566 .
C2 W1 C2 143.6(10) 10_554 .
C2 W1 C1 143.9(7) 20_657 10_554
C2 W1 C1 72.5(7) 27_566 10_554
C2 W1 C1 75.3(4) 10_554 10_554
C2 W1 C1 75.3(4) . 10_554
C2 W1 C1 75.3(4) 20_657 20_657
C2 W1 C1 75.3(4) 27_566 20_657
C2 W1 C1 72.5(7) 10_554 20_657
C2 W1 C1 143.9(7) . 20_657
C1 W1 C1 131.2(6) 10_554 20_657
C2 W1 C1 75.3(4) 20_657 27_566
C2 W1 C1 75.3(4) 27_566 27_566
C2 W1 C1 143.9(7) 10_554 27_566
C2 W1 C1 72.5(7) . 27_566
C1 W1 C1 131.2(6) 10_554 27_566
C1 W1 C1 71.4(9) 20_657 27_566
C2 W1 C1 72.5(7) 20_657 .
C2 W1 C1 143.9(7) 27_566 .
C2 W1 C1 75.3(4) 10_554 .
C2 W1 C1 75.3(4) . .
C1 W1 C1 71.4(9) 10_554 .
C1 W1 C1 131.2(6) 20_657 .
C1 W1 C1 131.2(6) 27_566 .
N2 Fe1 N2 180.0 . 17_656
N2 Fe1 N4 90.000(2) . .
N2 Fe1 N4 90.000(1) 17_656 .
N2 Fe1 N4 90.000(1) . 17_656
N2 Fe1 N4 90.000(2) 17_656 17_656
N4 Fe1 N4 180.0 . 17_656
N2 Fe1 N3 91(2) . 17_656
N2 Fe1 N3 89(2) 17_656 17_656
N4 Fe1 N3 90.000(2) . 17_656
N4 Fe1 N3 90.000(6) 17_656 17_656
N2 Fe1 N3 89(2) . .
N2 Fe1 N3 91(2) 17_656 .
N4 Fe1 N3 90.000(6) . .
N4 Fe1 N3 90.000(2) 17_656 .
N3 Fe1 N3 180.0 17_656 .
C2 N2 Fe1 176.3(17) . .
C3 N4 C3 120(3) . 6_556
C3 N4 Fe1 120.2(16) . .
C3 N4 Fe1 120.2(16) 6_556 .
C6 O2 H2A 154.3 . .
N1 C1 W1 176.5(17) . .
N2 C2 W1 179.7(18) . .
N4 C3 C4 119(3) . .
N4 C3 H3 120.3 . .
C4 C3 H3 120.3 . .
C5 C4 C3 118(3) . .
C5 C4 C6 129(4) . .
C3 C4 C6 110(4) . .
C4 C5 C4 126(5) . 6_556
C4 C5 H5 117.1 . .
C4 C5 H5 117.1 6_556 .
O2 C6 C4 147(5) . .
O2 C6 H12A 100.0 . .
C4 C6 H12A 100.0 . .
O2 C6 H12B 100.0 . .
C4 C6 H12B 100.0 . .
H12A C6 H12B 104.2 . .
C11 N3 C7 115(4) . .
C11 N3 Fe1 119(5) . .
C7 N3 Fe1 126(5) . .
N3 C11 C10 119(2) . 22_655
N3 C11 C10 119(2) . .
C10 C11 C10 67(7) 22_655 .
N3 C7 C8 116(4) . .
C10 C9 C8 113.4(18) . .
C10 C9 C9 86(3) . 22_655
C8 C9 C9 51(3) . 22_655
C11 C10 C9 114.5(18) . .
C11 C10 C12 96(6) . .
C9 C10 C12 117(8) . .
C11 C10 C10 56(3) . 22_655
C9 C10 C10 94(3) . 22_655
C12 C10 C10 59(3) . 22_655
C7 C8 C9 114(2) . 22_655
C7 C8 C9 114(2) . .
C9 C8 C9 78(6) 22_655 .
C10 C12 C10 62(6) . 22_655
C10 C12 O1 97(2) . .
C10 C12 O1 158(6) 22_655 .
C10 C12 O1 158(6) . 10_554
C10 C12 O1 97(2) 22_655 10_554
O1 C12 O1 104(6) . 10_554
C10 C12 C12 149(3) . 10_554
C10 C12 C12 149(3) 22_655 10_554
O1 C12 C12 53(3) . 10_554
O1 C12 C12 53(3) 10_554 10_554
C12 O1 C12 74(6) 10_554 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 C2 2.143(17) 20_657
W1 C2 2.143(17) 27_566
W1 C2 2.143(17) 10_554
W1 C2 2.143(17) .
W1 C1 2.15(2) 10_554
W1 C1 2.15(2) 20_657
W1 C1 2.15(2) 27_566
W1 C1 2.15(2) .
Fe1 N2 2.096(19) .
Fe1 N2 2.096(19) 17_656
Fe1 N4 2.15(3) .
Fe1 N4 2.15(3) 17_656
Fe1 N3 2.23(5) 17_656
Fe1 N3 2.23(5) .
N1 C1 1.17(2) .
N2 C2 1.12(2) .
N4 C3 1.35(3) .
N4 C3 1.35(3) 6_556
O2 C6 1.42(2) .
O2 H2A 1.0699 .
C3 C4 1.40(4) .
C3 H3 0.9300 .
C4 C5 1.29(4) .
C4 C6 1.50(2) .
C5 C4 1.29(4) 6_556
C5 H5 0.9300 .
C6 H12A 0.9700 .
C6 H12B 0.9700 .
N3 C11 1.37(2) .
N3 C7 1.37(2) .
C11 C10 1.405(18) 22_655
C11 C10 1.405(18) .
C7 C8 1.40(2) .
C9 C10 1.407(19) .
C9 C8 1.412(19) .
C9 C9 1.77(12) 22_655
C10 C12 1.51(2) .
C10 C10 1.56(14) 22_655
C8 C9 1.412(19) 22_655
C12 C10 1.51(2) 22_655
C12 O1 1.517(19) .
C12 O1 1.517(19) 10_554
C12 C12 1.83(13) 10_554
O1 C12 1.517(19) 10_554
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C3 N4 C3 C4 -2(3) 6_556 .
Fe1 N4 C3 C4 178(3) . .
N4 C3 C4 C5 5(5) . .
N4 C3 C4 C6 165(3) . .
C3 C4 C5 C4 -2(3) . 6_556
C6 C4 C5 C4 -158(6) . 6_556
C5 C4 C6 O2 107(11) . .
C3 C4 C6 O2 -50(11) . .
C7 N3 C11 C10 39(4) . 22_655
Fe1 N3 C11 C10 -141(4) . 22_655
C7 N3 C11 C10 -39(4) . .
Fe1 N3 C11 C10 141(4) . .
C11 N3 C7 C8 0.000(3) . .
Fe1 N3 C7 C8 180.000(7) . .
N3 C11 C10 C9 33(8) . .
C10 C11 C10 C9 -78(6) 22_655 .
N3 C11 C10 C12 157(5) . .
C10 C11 C10 C12 46(6) 22_655 .
N3 C11 C10 C10 112(3) . 22_655
C8 C9 C10 C11 11(8) . .
C9 C9 C10 C11 55(5) 22_655 .
C8 C9 C10 C12 -101(6) . .
C9 C9 C10 C12 -57(4) 22_655 .
C8 C9 C10 C10 -44(5) . 22_655
C9 C9 C10 C10 -0.001(6) 22_655 22_655
N3 C7 C8 C9 -43(3) . 22_655
N3 C7 C8 C9 43(3) . .
C10 C9 C8 C7 -48(7) . .
C9 C9 C8 C7 -111(3) 22_655 .
C10 C9 C8 C9 63(6) . 22_655
C11 C10 C12 C10 -44(6) . 22_655
C9 C10 C12 C10 78(6) . 22_655
C11 C10 C12 O1 141(4) . .
C9 C10 C12 O1 -97(6) . .
C10 C10 C12 O1 -175(6) 22_655 .
C11 C10 C12 O1 -58(21) . 10_554
C9 C10 C12 O1 64(21) . 10_554
C10 C10 C12 O1 -14(17) 22_655 10_554
C11 C10 C12 C12 128(6) . 10_554
C9 C10 C12 C12 -110(7) . 10_554
C10 C10 C12 C12 172(10) 22_655 10_554
C10 C12 O1 C12 -172(4) . 10_554
C10 C12 O1 C12 176(17) 22_655 10_554
O1 C12 O1 C12 15(7) 10_554 10_554
