#------------------------------------------------------------------------------
#$Date: 2023-10-06 02:51:31 +0300 (Fri, 06 Oct 2023) $
#$Revision: 286711 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/96/1569688.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_1569688
loop_
_publ_author_name
'Magott, Michał'
'Płonka, Klaudia'
'Sieklucka, Barbara'
'Dziedzic-Kocurek, Katarzyna'
'Kosaka, Wataru'
'Miyasaka, Hitoshi'
'Pinkowicz, Dawid'
_publ_section_title
;
 Guest-induced pore breathing controls the spin state in a cyanido-bridged
 framework.
;
_journal_issue                   36
_journal_name_full               'Chemical science'
_journal_page_first              9651
_journal_page_last               9663
_journal_paper_doi               10.1039/d3sc03255h
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C56 H32 Fe2 N24 W, 4(H2 O)'
_chemical_formula_sum            'C56 H40 Fe2 N24 O4 W'
_chemical_formula_weight         1408.67
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-09-12
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-07 deposited with the CCDC.	2023-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.7947(3)
_cell_length_b                   19.7947(3)
_cell_length_c                   16.0477(3)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.63
_cell_volume                     6287.97(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30445
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.858
_diffrn_reflns_theta_min         2.628
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.344
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0590 before and 0.0485 after correction.
The Ratio of minimum to maximum transmission is 0.8856.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       prism
_exptl_crystal_F_000             2808
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         3744
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0201
_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)+(0.0274P)²+8.2190P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0523
_refine_ls_wR_factor_ref         0.0535
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3458
_reflns_number_total             3744
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3sc03255h2.cif
_cod_data_source_block           fe2w_200k_0m
_cod_depositor_comments
'Adding full bibliography for 1569688--1569691.cif.'
_cod_original_cell_volume        6288.0(2)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               1569688
_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_max   0.835
_shelx_estimated_absorpt_t_min   0.603
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H,H) groups
2. Restrained distances
 O1-H1A
 0.95 with sigma of 0.02
 O1-H1B
 0.95 with sigma of 0.02
 H1A-H1B
 1.5 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C13(H13), C12(H12)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/4, x+3/4, z+3/4'
'y+1/4, -x+1/4, z+1/4'
'-x, -y+1/2, z'
'x+1/2, y+1/2, z+1/2'
'-y+3/4, x+5/4, z+5/4'
'y+3/4, -x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'-x, -y, -z'
'y-1/4, -x-3/4, -z-3/4'
'-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'
'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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.5000 0.7500 0.6250 0.01676(5) Uani 1 4 d S T P . .
O1 O 0.4224(2) 0.9264(2) 0.9053(2) 0.1265(15) Uani 1 1 d D . . . .
H1A H 0.450(2) 0.926(3) 0.956(2) 0.152 Uiso 1 1 d D U . . .
H1B H 0.438(3) 0.891(2) 0.869(3) 0.152 Uiso 1 1 d D U . . .
N1 N 0.48987(11) 0.59432(9) 0.55576(12) 0.0377(5) Uani 1 1 d . . . . .
C1 C 0.49306(11) 0.64807(10) 0.58336(13) 0.0263(4) Uani 1 1 d . . . . .
Fe1 Fe 0.5000 0.5000 0.5000 0.03312(10) Uani 1 2 d S . P . .
C2 C 0.50287(11) 0.81602(11) 0.73310(13) 0.0286(4) Uani 1 1 d . . . . .
N3 N 0.49382(12) 0.45210(10) 0.62645(12) 0.0398(5) Uani 1 1 d . . . . .
C3 C 0.50712(16) 0.48839(13) 0.69478(16) 0.0463(6) Uani 1 1 d . . . . .
H3 H 0.5225 0.5335 0.6877 0.056 Uiso 1 1 calc R U . . .
N4 N 0.4637(2) 0.35202(19) 0.93445(19) 0.0960(12) Uani 1 1 d . . . . .
C4 C 0.49991(17) 0.46455(15) 0.77447(17) 0.0519(7) Uani 1 1 d . . . . .
H4 H 0.5101 0.4922 0.8212 0.062 Uiso 1 1 calc R U . . .
C5 C 0.47739(17) 0.39894(15) 0.78463(17) 0.0529(7) Uani 1 1 d . . . . .
N5 N 0.38708(12) 0.49360(11) 0.48176(14) 0.0461(5) Uani 1 1 d . . . . .
N2 N 0.50343(13) 0.85172(11) 0.78936(14) 0.0462(5) Uani 1 1 d . . . . .
C6 C 0.4636(2) 0.35985(15) 0.71572(19) 0.0668(10) Uani 1 1 d . . . . .
H6 H 0.4481 0.3146 0.7213 0.080 Uiso 1 1 calc R U . . .
N6 N 0.1198(2) 0.4841(3) 0.4233(3) 0.1259(17) Uani 1 1 d . . . . .
C7 C 0.4730(2) 0.38855(14) 0.63834(17) 0.0590(9) Uani 1 1 d . . . . .
H7 H 0.4641 0.3616 0.5906 0.071 Uiso 1 1 calc R U . . .
C8 C 0.4691(2) 0.37210(19) 0.8682(2) 0.0691(10) Uani 1 1 d . . . . .
C9 C 0.3507(2) 0.54921(17) 0.4696(3) 0.0748(11) Uani 1 1 d . . . . .
H9 H 0.3733 0.5916 0.4713 0.090 Uiso 1 1 calc R U . . .
C10 C 0.2821(2) 0.5489(2) 0.4547(3) 0.0845(12) Uani 1 1 d . . . . .
H10 H 0.2585 0.5901 0.4461 0.101 Uiso 1 1 calc R U . . .
C11 C 0.24830(18) 0.48862(19) 0.4525(2) 0.0636(8) Uani 1 1 d . . . . .
C13 C 0.35284(17) 0.43530(16) 0.4781(2) 0.0648(9) Uani 1 1 d . . . . .
H13 H 0.3774 0.3945 0.4854 0.078 Uiso 1 1 calc R U . . .
C14 C 0.1764(2) 0.4862(2) 0.4365(3) 0.0871(13) Uani 1 1 d . . . . .
C12 C 0.28428(19) 0.43082(18) 0.4645(3) 0.0737(10) Uani 1 1 d . . . . .
H12 H 0.2625 0.3881 0.4636 0.088 Uiso 1 1 calc R U . . .
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
_geom_angle_publ_flag
C1 W1 C1 95.65(3) 15_656 4_665 ?
C1 W1 C1 143.44(11) 4_665 . ?
C1 W1 C1 95.65(3) 15_656 . ?
C1 W1 C1 143.44(11) 15_656 10_577 ?
C1 W1 C1 95.65(3) 4_665 10_577 ?
C1 W1 C1 95.65(3) 10_577 . ?
C1 W1 C2 145.28(8) 10_577 10_577 ?
C1 W1 C2 145.28(8) . . ?
C1 W1 C2 71.27(8) 4_665 . ?
C1 W1 C2 145.28(8) 4_665 4_665 ?
C1 W1 C2 74.66(8) 4_665 10_577 ?
C1 W1 C2 71.28(8) . 4_665 ?
C1 W1 C2 74.66(8) 15_656 4_665 ?
C1 W1 C2 145.28(8) 15_656 15_656 ?
C1 W1 C2 76.33(8) 10_577 4_665 ?
C1 W1 C2 76.33(8) 4_665 15_656 ?
C1 W1 C2 76.33(8) 15_656 . ?
C1 W1 C2 71.27(8) 10_577 15_656 ?
C1 W1 C2 74.66(8) 10_577 . ?
C1 W1 C2 74.66(8) . 15_656 ?
C1 W1 C2 71.27(8) 15_656 10_577 ?
C1 W1 C2 76.32(8) . 10_577 ?
C2 W1 C2 129.61(7) 10_577 4_665 ?
C2 W1 C2 74.03(11) 15_656 10_577 ?
C2 W1 C2 129.61(7) 10_577 . ?
C2 W1 C2 74.03(11) 4_665 . ?
C2 W1 C2 129.61(7) 15_656 . ?
C2 W1 C2 129.61(7) 15_656 4_665 ?
H1A O1 H1B 108(3) . . ?
C1 N1 Fe1 170.8(2) . . ?
N1 C1 W1 175.69(19) . . ?
N1 Fe1 N1 180.0 . 9_666 ?
N1 Fe1 N3 90.86(7) . 9_666 ?
N1 Fe1 N3 90.86(7) 9_666 . ?
N1 Fe1 N3 89.14(7) . . ?
N1 Fe1 N3 89.13(7) 9_666 9_666 ?
N1 Fe1 N5 90.62(8) . . ?
N1 Fe1 N5 89.38(8) . 9_666 ?
N1 Fe1 N5 89.38(8) 9_666 . ?
N1 Fe1 N5 90.62(8) 9_666 9_666 ?
N3 Fe1 N3 180.0 9_666 . ?
N3 Fe1 N5 87.73(9) . 9_666 ?
N3 Fe1 N5 92.27(9) . . ?
N3 Fe1 N5 87.73(9) 9_666 . ?
N3 Fe1 N5 92.27(9) 9_666 9_666 ?
N5 Fe1 N5 180.0 . 9_666 ?
N2 C2 W1 178.6(2) . . ?
C3 N3 Fe1 120.27(17) . . ?
C3 N3 C7 116.7(2) . . ?
C7 N3 Fe1 122.92(17) . . ?
N3 C3 H3 118.0 . . ?
N3 C3 C4 124.0(3) . . ?
C4 C3 H3 118.0 . . ?
C3 C4 H4 121.1 . . ?
C3 C4 C5 117.8(3) . . ?
C5 C4 H4 121.1 . . ?
C4 C5 C8 119.3(3) . . ?
C6 C5 C4 119.8(3) . . ?
C6 C5 C8 120.9(3) . . ?
C9 N5 Fe1 120.6(2) . . ?
C9 N5 C13 115.7(3) . . ?
C13 N5 Fe1 123.7(2) . . ?
C5 C6 H6 121.1 . . ?
C5 C6 C7 117.7(3) . . ?
C7 C6 H6 121.1 . . ?
N3 C7 C6 123.9(3) . . ?
N3 C7 H7 118.0 . . ?
C6 C7 H7 118.0 . . ?
N4 C8 C5 178.4(5) . . ?
N5 C9 H9 118.2 . . ?
N5 C9 C10 123.7(3) . . ?
C10 C9 H9 118.2 . . ?
C9 C10 H10 120.3 . . ?
C11 C10 C9 119.4(3) . . ?
C11 C10 H10 120.3 . . ?
C10 C11 C14 120.9(4) . . ?
C12 C11 C10 118.2(3) . . ?
C12 C11 C14 120.8(4) . . ?
N5 C13 H13 117.9 . . ?
N5 C13 C12 124.1(3) . . ?
C12 C13 H13 117.9 . . ?
N6 C14 C11 179.5(6) . . ?
C11 C12 C13 118.9(3) . . ?
C11 C12 H12 120.5 . . ?
C13 C12 H12 120.5 . . ?
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
W1 C1 2.130(2) 15_656 ?
W1 C1 2.130(2) 10_577 ?
W1 C1 2.130(2) 4_665 ?
W1 C1 2.130(2) . ?
W1 C2 2.173(2) 10_577 ?
W1 C2 2.173(2) . ?
W1 C2 2.173(2) 4_665 ?
W1 C2 2.173(2) 15_656 ?
O1 H1A 0.982(19) . ?
O1 H1B 0.969(19) . ?
N1 C1 1.154(3) . ?
N1 Fe1 2.0800(18) . ?
Fe1 N1 2.0801(18) 9_666 ?
Fe1 N3 2.2431(19) . ?
Fe1 N3 2.2430(19) 9_666 ?
Fe1 N5 2.258(2) 9_666 ?
Fe1 N5 2.258(2) . ?
C2 N2 1.147(3) . ?
N3 C3 1.337(3) . ?
N3 C7 1.338(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.371(4) . ?
N4 C8 1.139(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.383(4) . ?
C5 C6 1.377(4) . ?
C5 C8 1.452(4) . ?
N5 C9 1.330(4) . ?
N5 C13 1.340(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.378(4) . ?
N6 C14 1.142(5) . ?
C7 H7 0.9500 . ?
C9 H9 0.9500 . ?
C9 C10 1.379(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.368(5) . ?
C11 C14 1.446(5) . ?
C11 C12 1.362(5) . ?
C13 H13 0.9500 . ?
C13 C12 1.377(5) . ?
C12 H12 0.9500 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N3 C3 C4 175.2(2) . . . . ?
Fe1 N3 C7 C6 -174.6(3) . . . . ?
Fe1 N5 C9 C10 177.3(4) . . . . ?
Fe1 N5 C13 C12 -178.0(3) . . . . ?
N3 C3 C4 C5 -0.1(5) . . . . ?
C3 N3 C7 C6 1.2(5) . . . . ?
C3 C4 C5 C6 0.5(5) . . . . ?
C3 C4 C5 C8 -179.9(3) . . . . ?
C4 C5 C6 C7 -0.1(6) . . . . ?
C5 C6 C7 N3 -0.9(6) . . . . ?
N5 C9 C10 C11 0.4(7) . . . . ?
N5 C13 C12 C11 1.1(6) . . . . ?
C7 N3 C3 C4 -0.8(5) . . . . ?
C8 C5 C6 C7 -179.6(4) . . . . ?
C9 N5 C13 C12 -1.2(6) . . . . ?
C9 C10 C11 C14 -179.6(4) . . . . ?
C9 C10 C11 C12 -0.6(7) . . . . ?
C10 C11 C12 C13 -0.2(6) . . . . ?
C13 N5 C9 C10 0.4(6) . . . . ?
C14 C11 C12 C13 178.9(4) . . . . ?
