#------------------------------------------------------------------------------
#$Date: 2017-01-09 05:17:38 +0200 (Mon, 09 Jan 2017) $
#$Revision: 190118 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/10/7041020.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_7041020
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
;
2016-10-07 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                   20.2282(6)
_cell_length_b                   20.2282(6)
_cell_length_c                   13.8297(8)
_cell_measurement_reflns_used    11768
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.8
_cell_measurement_theta_min      2.18
_cell_volume                     5658.8(4)
_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 0.996
_diffrn_measured_fraction_theta_max 0.997
_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  0.0533
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22827
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.561
_diffrn_reflns_theta_min         2.014
_exptl_absorpt_coefficient_mu    2.604
_exptl_absorpt_correction_T_max  0.594
_exptl_absorpt_correction_T_min  0.541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2776
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.226
_refine_diff_density_min         -1.238
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1734
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0209P)²+62.2959P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0747
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1671
_reflns_number_total             1734
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt03421g2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7041017--7041023.cif.'
_cod_original_cell_volume        5658.8(5)
_cod_database_code               7041020
_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   0.562
_shelx_estimated_absorpt_t_max   0.624
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
C1 C 0.4370(2) 0.2500 0.4976(3) 0.0193(9) Uani 1 2 d S T P
C2 C 0.5000 0.1496(2) 0.5812(3) 0.0192(9) Uani 1 2 d S T P
C3 C 0.3534(3) 0.0567(3) 0.4969(3) 0.0450(11) Uani 1 1 d . . .
H3 H 0.3762 0.0966 0.4944 0.054 Uiso 1 1 calc R U .
C4 C 0.2846(3) 0.0581(3) 0.4974(4) 0.0557(14) Uani 1 1 d . . .
H4 H 0.2624 0.0984 0.4959 0.067 Uiso 1 1 calc R U .
C5 C 0.2495(4) 0.0000 0.5000 0.057(2) Uani 1 2 d S T P
C6 C 0.1715(5) 0.0000 0.5000 0.078(3) Uani 1 2 d DS T P
H6A H 0.1547 0.0366 0.5368 0.094 Uiso 0.5 1 d R U P
H6B H 0.1547 0.0029 0.4352 0.094 Uiso 0.5 1 d R U P
C7 C 0.5000 0.0035(3) 0.2733(4) 0.055(2) Uani 1 2 d S T P
H7 H 0.5000 -0.0420 0.2830 0.066 Uiso 1 2 calc R U P
C8 C 0.5000 0.0262(3) 0.1779(4) 0.0430(16) Uani 1 2 d S T P
H8 H 0.5000 -0.0037 0.1268 0.052 Uiso 1 2 calc R U P
C9 C 0.5000 0.0902(4) 0.1608(5) 0.074(3) Uani 1 2 d DS T P
C10 C 0.5000 0.1304(5) 0.2397(7) 0.097(3) Uani 1 2 d S TU P
H10 H 0.5000 0.1760 0.2312 0.117 Uiso 1 2 calc R U P
C11 C 0.5000 0.1046(4) 0.3317(5) 0.082(4) Uani 1 2 d S T P
H11 H 0.5000 0.1337 0.3838 0.099 Uiso 1 2 calc R U P
C12 C 0.5245(5) 0.1190(6) 0.0607(6) 0.050(2) Uani 0.5 1 d D . P
H12A H 0.5683 0.1046 0.0447 0.060 Uiso 0.5 1 d R U P
H12B H 0.5227 0.1664 0.0603 0.060 Uiso 0.5 1 d R U P
Fe1 Fe 0.5000 0.0000 0.5000 0.0246(2) Uani 1 4 d S T P
N1 N 0.4041(2) 0.2500 0.4292(3) 0.0316(11) Uani 1 2 d S T P
N2 N 0.5000 0.0952(2) 0.5559(3) 0.0310(11) Uani 1 2 d S T P
N3 N 0.5000 0.0412(2) 0.3496(3) 0.0288(10) Uani 1 2 d S T P
N4 N 0.3884(3) 0.0000 0.5000 0.0368(11) Uani 1 2 d S T P
O1 O 0.1559(5) -0.0606(3) 0.5442(7) 0.102(4) Uani 0.5 1 d D . P
H1C H 0.1160 -0.0696 0.5298 0.122 Uiso 0.5 1 d R U P
O2 O 0.4772(3) 0.0919(3) -0.0011(5) 0.0514(19) Uani 0.5 1 d D U P
H2C H 0.4818 0.1090 -0.0569 0.062 Uiso 0.5 1 d R U P
W1 W 0.5000 0.2500 0.6250 0.00903(10) Uani 1 8 d S T 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
N1 C1 W1 179.2(4) . .
N2 C2 W1 178.9(4) . .
N4 C3 C4 122.8(5) . .
N4 C3 H3 118.6 . .
C4 C3 H3 118.6 . .
C5 C4 C3 119.9(6) . .
C5 C4 H4 120.0 . .
C3 C4 H4 120.0 . .
C4 C5 C4 117.8(7) . 6_556
C4 C5 C6 121.1(4) . .
C4 C5 C6 121.1(4) 6_556 .
O1 C6 O1 154.0(13) . 6_556
O1 C6 C5 103.0(7) . .
O1 C6 C5 103.0(7) 6_556 .
O1 C6 H6A 111.2 . .
O1 C6 H6A 58.6 6_556 .
C5 C6 H6A 110.7 . .
O1 C6 H6B 112.2 . .
O1 C6 H6B 57.5 6_556 .
C5 C6 H6B 110.7 . .
H6A C6 H6B 108.8 . .
N3 C7 C8 125.0(6) . .
N3 C7 H7 117.5 . .
C8 C7 H7 117.5 . .
C9 C8 C7 119.5(6) . .
C9 C8 H8 120.2 . .
C7 C8 H8 120.2 . .
C8 C9 C10 116.4(7) . .
C8 C9 C12 121.3(7) . .
C10 C9 C12 118.7(8) . .
C8 C9 C12 121.3(7) . 22_655
C10 C9 C12 118.7(8) . 22_655
C12 C9 C12 36.4(7) . 22_655
C9 C10 C11 120.9(8) . .
C9 C10 H10 119.5 . .
C11 C10 H10 119.5 . .
N3 C11 C10 123.2(7) . .
N3 C11 H11 118.4 . .
C10 C11 H11 118.4 . .
C12 C12 O2 88.1(7) 22_655 22_655
C12 C12 O2 46.7(5) 22_655 .
O2 C12 O2 41.4(7) 22_655 .
C12 C12 C9 71.8(3) 22_655 .
O2 C12 C9 121.9(11) 22_655 .
O2 C12 C9 100.2(7) . .
C12 C12 H12A 157.6 22_655 .
O2 C12 H12A 70.9 22_655 .
O2 C12 H12A 112.0 . .
C9 C12 H12A 112.3 . .
C12 C12 H12B 87.8 22_655 .
O2 C12 H12B 122.2 22_655 .
O2 C12 H12B 111.3 . .
C9 C12 H12B 111.2 . .
H12A C12 H12B 109.6 . .
N2 Fe1 N2 180.0 17_656 .
N2 Fe1 N3 90.08(16) 17_656 17_656
N2 Fe1 N3 89.93(16) . 17_656
N2 Fe1 N3 89.93(16) 17_656 .
N2 Fe1 N3 90.07(16) . .
N3 Fe1 N3 180.0 17_656 .
N2 Fe1 N4 90.0 17_656 17_656
N2 Fe1 N4 90.0 . 17_656
N3 Fe1 N4 90.0 17_656 17_656
N3 Fe1 N4 90.0 . 17_656
N2 Fe1 N4 90.0 17_656 .
N2 Fe1 N4 90.0 . .
N3 Fe1 N4 90.0 17_656 .
N3 Fe1 N4 90.0 . .
N4 Fe1 N4 180.0 17_656 .
C2 N2 Fe1 175.8(4) . .
C7 N3 C11 114.9(5) . .
C7 N3 Fe1 122.4(4) . .
C11 N3 Fe1 122.7(4) . .
C3 N4 C3 116.7(6) 6_556 .
C3 N4 Fe1 121.7(3) 6_556 .
C3 N4 Fe1 121.7(3) . .
C6 O1 H1C 107.4 . .
O2 O2 C12 91.9(7) 22_655 22_655
O2 O2 C12 46.7(5) 22_655 .
C12 O2 C12 45.2(9) 22_655 .
O2 O2 H2C 83.7 22_655 .
C12 O2 H2C 123.2 22_655 .
C12 O2 H2C 108.7 . .
C2 W1 C2 146.8(2) 20_657 27_566
C2 W1 C2 94.67(6) 20_657 10_554
C2 W1 C2 94.67(6) 27_566 10_554
C2 W1 C2 94.67(6) 20_657 .
C2 W1 C2 94.67(6) 27_566 .
C2 W1 C2 146.8(2) 10_554 .
C2 W1 C1 142.48(16) 20_657 .
C2 W1 C1 70.70(17) 27_566 .
C2 W1 C1 76.63(9) 10_554 .
C2 W1 C1 76.63(9) . .
C2 W1 C1 76.63(9) 20_657 27_566
C2 W1 C1 76.63(9) 27_566 27_566
C2 W1 C1 70.70(17) 10_554 27_566
C2 W1 C1 142.48(16) . 27_566
C1 W1 C1 131.02(15) . 27_566
C2 W1 C1 76.63(9) 20_657 20_657
C2 W1 C1 76.63(9) 27_566 20_657
C2 W1 C1 142.48(16) 10_554 20_657
C2 W1 C1 70.70(17) . 20_657
C1 W1 C1 131.02(15) . 20_657
C1 W1 C1 71.8(2) 27_566 20_657
C2 W1 C1 70.70(17) 20_657 10_554
C2 W1 C1 142.48(16) 27_566 10_554
C2 W1 C1 76.63(9) 10_554 10_554
C2 W1 C1 76.63(9) . 10_554
C1 W1 C1 71.8(2) . 10_554
C1 W1 C1 131.02(15) 27_566 10_554
C1 W1 C1 131.02(15) 20_657 10_554
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.155(6) .
C1 W1 2.175(5) .
C2 N2 1.153(6) .
C2 W1 2.120(5) .
C3 N4 1.349(6) .
C3 C4 1.393(7) .
C3 H3 0.9300 .
C4 C5 1.374(7) .
C4 H4 0.9300 .
C5 C4 1.374(7) 6_556
C5 C6 1.578(13) .
C6 O1 1.405(2) .
C6 O1 1.405(2) 6_556
C6 H6A 0.9600 .
C6 H6B 0.9601 .
C7 N3 1.301(7) .
C7 C8 1.396(8) .
C7 H7 0.9300 .
C8 C9 1.316(10) .
C8 H8 0.9300 .
C9 C10 1.361(13) .
C9 C12 1.582(10) .
C9 C12 1.582(10) 22_655
C10 C11 1.376(11) .
C10 H10 0.9300 .
C11 N3 1.307(8) .
C11 H11 0.9300 .
C12 C12 0.989(19) 22_655
C12 O2 1.016(10) 22_655
C12 O2 1.394(10) .
C12 H12A 0.9599 .
C12 H12B 0.9599 .
Fe1 N2 2.076(4) 17_656
Fe1 N2 2.076(4) .
Fe1 N3 2.241(4) 17_656
Fe1 N3 2.241(4) .
Fe1 N4 2.257(6) 17_656
Fe1 N4 2.257(6) .
N4 C3 1.348(6) 6_556
O1 H1C 0.8501 .
O2 O2 0.923(13) 22_655
O2 C12 1.015(10) 22_655
O2 H2C 0.8499 .
W1 C2 2.120(5) 20_657
W1 C2 2.120(5) 27_566
W1 C2 2.120(5) 10_554
W1 C1 2.175(5) 27_566
W1 C1 2.175(5) 20_657
W1 C1 2.175(5) 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
N4 C3 C4 C5 -0.7(7) . .
C3 C4 C5 C4 0.3(3) . 6_556
C3 C4 C5 C6 -179.7(3) . .
C4 C5 C6 O1 -155.3(5) . .
C4 C5 C6 O1 24.7(5) 6_556 .
C4 C5 C6 O1 24.7(5) . 6_556
C4 C5 C6 O1 -155.3(5) 6_556 6_556
N3 C7 C8 C9 0.000(1) . .
C7 C8 C9 C10 0.000(1) . .
C7 C8 C9 C12 158.5(4) . .
C7 C8 C9 C12 -158.5(4) . 22_655
C8 C9 C10 C11 0.000(1) . .
C12 C9 C10 C11 -159.1(4) . .
C12 C9 C10 C11 159.1(4) 22_655 .
C9 C10 C11 N3 0.000(1) . .
C8 C9 C12 C12 101.5(4) . 22_655
C10 C9 C12 C12 -100.4(4) . 22_655
C8 C9 C12 O2 25.7(12) . 22_655
C10 C9 C12 O2 -176.2(9) . 22_655
C12 C9 C12 O2 -75.8(11) 22_655 22_655
C8 C9 C12 O2 64.0(7) . .
C10 C9 C12 O2 -137.9(5) . .
C12 C9 C12 O2 -37.5(7) 22_655 .
C8 C7 N3 C11 0.000(1) . .
C8 C7 N3 Fe1 180.000(0) . .
C10 C11 N3 C7 0.000(1) . .
C10 C11 N3 Fe1 180.000(1) . .
C4 C3 N4 C3 0.3(3) . 6_556
C4 C3 N4 Fe1 -179.7(3) . .
C12 C12 O2 O2 180.004(1) 22_655 22_655
C9 C12 O2 O2 -127.3(9) . 22_655
O2 C12 O2 C12 179.996(1) 22_655 22_655
C9 C12 O2 C12 52.7(9) . 22_655
