#------------------------------------------------------------------------------
#$Date: 2019-11-23 14:17:16 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233581 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/91/4349105.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_4349105
loop_
_publ_author_name
'Valverde-Mu\~noz, Francisco Javier'
'Seredyuk, Maksym'
'Mu\~noz, M Carmen'
'Znovjyak, Kateryna'
'Fritsky, Igor O.'
'Real, Jos\'e Antonio'
_publ_section_title
;
Strong Cooperative Spin Crossover in 2D and 3D
FeII-MI,II Hofmann-Like Coordination Polymers Based
on 2-Fluoropyrazine.
;
_journal_issue 20
_journal_name_full 'Inorganic chemistry'
_journal_page_first 10654
_journal_page_last 10665
_journal_paper_doi 10.1021/acs.inorgchem.6b01901
_journal_volume 55
_journal_year 2016
_chemical_formula_sum 'C12 H6 F2 Fe N8 Pt'
_chemical_formula_weight 551.19
_space_group_crystal_system orthorhombic
_space_group_IT_number 53
_space_group_name_Hall '-P 2ac 2'
_space_group_name_H-M_alt 'P m n a'
_atom_sites_solution_hydrogens geom
_audit_creation_method SHELXL-2014
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 7.2572(3)
_cell_length_b 6.9861(3)
_cell_length_c 14.9922(6)
_cell_measurement_reflns_used 2798
_cell_measurement_temperature 120(1)
_cell_measurement_theta_max 29.7210
_cell_measurement_theta_min 3.2030
_cell_volume 760.10(5)
_computing_cell_refinement 'CrysAlisPro 2015'
_computing_data_collection 'CrysAlisPro 2015'
_computing_data_reduction 'CrysAlisPro 2015'
_computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution 'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature 120(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type 'SuperNova Sapphire3'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0384
_diffrn_reflns_av_unetI/netI 0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max 5
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 6092
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full 25.000
_diffrn_reflns_theta_max 29.978
_diffrn_reflns_theta_min 2.916
_exptl_absorpt_coefficient_mu 10.181
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.65771
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'CrysAlisPro 1.171.38.41q'
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 2.408
_exptl_crystal_description prismatic
_exptl_crystal_F_000 512
_exptl_crystal_size_max 0.100
_exptl_crystal_size_mid 0.100
_exptl_crystal_size_min 0.060
_refine_diff_density_max 1.122
_refine_diff_density_min -0.771
_refine_diff_density_rms 0.152
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.951
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 69
_refine_ls_number_reflns 1091
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.951
_refine_ls_R_factor_all 0.0318
_refine_ls_R_factor_gt 0.0200
_refine_ls_shift/su_max 0.016
_refine_ls_shift/su_mean 0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+0.9728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0449
_refine_ls_wR_factor_ref 0.0509
_reflns_Friedel_coverage 0.000
_reflns_number_gt 816
_reflns_number_total 1091
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ic6b01901_si_005.cif
_cod_data_source_block shelx
_cod_database_code 4349105
_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 0.429
_shelx_estimated_absorpt_t_max 0.580
_shelxl_version_number 2014-1
_shelx_res_file
;
TITL ja1412 in Pnc2
CELL 0.71073 7.257230 6.986081 14.992222 90.0000 90.0000 90.0000
ZERR 2 0.000286 0.000262 0.000642 0.0000 0.0000 0.0000
LATT 1
SYMM 1/2 - X, - Y, 1/2 + Z
SYMM X, - Y, - Z
SYMM 1/2 - X, Y, 1/2 - Z
SFAC C H N F FE PT
UNIT 24 12 16 4 2 2
MERG 2
bond
bond $H
omit -3 180
acta 50
FMAP 2
PLAN 25
L.S. 4
size 0.06 0.10 0.10
WGHT 0.025400 0.972800
FVAR 3.64518
PT 6 0.500000 0.000000 0.500000 10.25000 0.00460 0.00451 =
0.01193 0.00016 0.00000 0.00000
FE 5 1.000000 0.500000 0.500000 10.25000 0.00426 0.00504 =
0.01326 0.00186 0.00000 0.00000
N1 3 1.000000 0.570056 0.371337 10.50000 0.00505 0.01213 =
0.01171 0.00271 0.00000 0.00000
N2 3 0.809404 0.309454 0.480868 11.00000 0.01010 0.01072 =
0.01748 0.00055 -0.00056 0.00181
N3 3 1.000000 0.672136 0.191260 10.50000 0.03926 0.02785 =
0.02046 0.00792 0.00000 0.00000
C1 1 1.000000 0.753398 0.345728 10.50000 0.02080 0.01575 =
0.01985 0.00214 0.00000 0.00000
AFIX 43
H1 2 1.000000 0.850911 0.387956 10.50000 -1.20000
AFIX 0
C2 1 1.000000 0.796071 0.255972 10.50000 0.03157 0.02264 =
0.02107 0.01113 0.00000 0.00000
C3 1 1.000000 0.488628 0.218467 10.50000 0.02984 0.02625 =
0.02713 -0.01320 0.00000 0.00000
AFIX 43
H3 2 1.000000 0.393078 0.175275 10.50000 -1.20000
AFIX 0
C4 1 1.000000 0.434745 0.306556 10.50000 0.01799 0.01381 =
0.02158 -0.00100 0.00000 0.00000
AFIX 43
H4 2 1.000000 0.305667 0.321729 10.50000 -1.20000
AFIX 0
C5 1 0.695143 0.197033 0.484233 11.00000 0.01098 0.00771 =
0.01738 0.00129 -0.00071 0.00145
F 4 1.000000 0.982690 0.231703 10.50000 0.09495 0.02258 =
0.02662 0.01261 0.00000 0.00000
HKLF 4
REM ja1412 in Pnc2
REM R1 = 0.0200 for 816 Fo > 4sig(Fo) and 0.0318 for all 1091 data
REM 69 parameters refined using 0 restraints
END
WGHT 0.0198 0.3108
REM Highest difference peak 1.122, deepest hole -0.771, 1-sigma level 0.152
Q1 1 0.5000 -0.0091 0.5587 10.50000 0.05 1.12
Q2 1 0.4506 0.0014 0.6093 11.00000 0.05 0.67
Q3 1 1.0000 0.9977 0.2819 10.50000 0.05 0.65
Q4 1 0.6327 0.1416 0.5030 11.00000 0.05 0.62
Q5 1 1.0000 1.0053 0.1717 10.50000 0.05 0.56
Q6 1 1.0000 0.6427 0.1381 10.50000 0.05 0.55
Q7 1 0.8808 0.3113 0.5031 11.00000 0.05 0.47
Q8 1 0.6929 0.0084 0.4194 11.00000 0.05 0.47
Q9 1 1.0000 0.3408 0.1331 10.50000 0.05 0.47
Q10 1 0.8048 0.2271 0.4595 11.00000 0.05 0.46
Q11 1 0.6381 0.0631 0.4641 11.00000 0.05 0.46
Q12 1 1.0000 1.0726 0.3500 10.50000 0.05 0.46
Q13 1 0.8215 0.0000 0.5000 10.50000 0.05 0.45
Q14 1 0.5000 0.2953 0.4623 10.50000 0.05 0.44
Q15 1 1.0000 0.4589 0.4416 10.50000 0.05 0.42
Q16 1 0.3781 0.0749 0.5437 11.00000 0.05 0.42
Q17 1 1.0485 0.5557 0.4232 11.00000 0.05 0.41
Q18 1 1.1958 0.6347 0.1137 11.00000 0.05 0.40
Q19 1 0.6661 0.5000 0.5000 10.50000 0.05 0.40
Q20 1 1.1164 0.5054 0.4654 11.00000 0.05 0.39
Q21 1 0.5000 0.3236 0.5286 10.50000 0.05 0.39
Q22 1 1.0000 0.2417 0.1625 10.50000 0.05 0.39
Q23 1 1.2226 0.2917 0.1537 11.00000 0.05 0.39
Q24 1 1.0000 0.9386 0.4267 10.50000 0.05 0.38
Q25 1 0.3396 -0.0211 0.5287 11.00000 0.05 0.38
;
_shelx_res_checksum 76383
_shelx_hkl_file
;
4 0 0 720138. 14948.8 4
3 0 0 63.8473 144.617 4
2 0 0 999999. 19032.1 4
2 0 0 980051. 20115.1 5
-2 0 0 991857. 19366.2 4
-3 0 0 71.8514 180.983 4
-4 0 0 736754. 18159.6 2
-4 0 0 694316. 15852.4 1
-4 0 0 735061. 15659.9 4
-5 0 0 111.937 294.177 1
-5 0 0-128.551 256.317 4
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-6 0 0 414892. 14289.4 2
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-6 0 0 430728. 11276.7 4
-7 0 0-254.040 768.148 2
-8 0 0 116115. 8113.67 2
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4 0 -1-66.2468 262.615 4
3 0 1 88802.8 2847.09 4
3 0 -1 85307.1 2577.14 4
2 0 -1-59.5334 93.3866 4
2 0 1 17.0694 166.968 4
2 0 -1-80.7747 152.339 3
2 0 -1 74.7214 173.465 5
1 0 -1 67648.3 1876.22 3
1 0 -1 68221.1 1912.53 5
1 0 1 67404.4 2024.76 4
-1 0 1 69134.8 1903.12 3
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-3 0 1 85984.7 2698.79 4
-4 0 1 14.6857 175.054 1
-4 0 -1 199.771 376.435 1
-4 0 1-50.2309 236.628 4
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-4 0 1-82.6134 399.494 2
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-5 0 -1 55929.5 4043.47 2
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-3 -7 4 1346.06 796.710 5
-4 -7 4 32614.2 4187.98 6
-4 -7 -4 26599.3 3626.31 6
-4 -7 4 32145.2 3453.51 5
-4 7 -4 39332.7 4284.00 4
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-5 7 -4-196.480 921.666 4
-5 7 4-403.268 653.263 4
-5 -7 4 1418.63 1261.83 6
-5 -7 -4-281.809 964.529 6
-5 -7 4 178.713 701.410 5
-6 -7 4 27853.7 3813.51 5
2 7 5 2671.64 862.730 4
1 7 -5 109786. 6310.92 4
1 7 5 111586. 5522.55 4
0 7 -5 28.5039 604.501 4
0 7 5 272.159 457.290 4
0 -7 5 270.505 418.941 5
-1 -7 5 119713. 5810.48 5
-1 7 -5 122967. 7078.20 4
-1 7 5 113882. 6025.47 4
-2 7 -5 3227.46 1319.97 4
-2 7 5 1159.24 723.456 4
-2 -7 5 2370.91 1263.30 6
-2 -7 -5 1853.27 974.014 6
-2 -7 5 618.433 607.561 5
-3 -7 5 135013. 8307.27 6
-3 -7 -5 131580. 8084.30 6
-3 -7 5 122256. 6650.27 5
-3 7 -5 138484. 8115.70 4
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-4 7 -5 192.860 759.724 4
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-4 -7 5 1610.89 1169.26 6
-4 -7 -5 311.114 851.170 6
-4 -7 5 133.261 557.387 5
-5 -7 5 68410.9 6309.63 6
-5 -7 -5 66704.4 6048.57 6
-5 -7 5 73978.1 5747.75 5
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2 7 6 52822.5 3589.89 4
1 7 -6 351.209 607.608 4
1 7 6 154.319 608.780 4
0 -7 6 44457.8 3423.48 5
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1 7 -7 110610. 6899.25 4
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-3 -7 -8 690.492 815.983 6
-3 -7 8 245.205 619.258 5
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-4 -7 -8 24974.7 3515.39 6
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0 -8 7 897.964 694.799 5
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0 9 -3-1208.33 1035.87 4
0 9 3-21.6023 749.097 4
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0 9 4 36484.9 3780.25 4
-1 9 -4-789.052 1002.49 4
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0 9 5 838.922 714.907 4
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0 9 6 32498.1 3618.83 4
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0 9 7 2186.24 1037.54 4
-1 9 -7 77871.4 6925.66 4
0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 10577
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x, -y, -z'
'-x+1/2, y, -z+1/2'
'-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pt Pt 0.5000 0.0000 0.5000 0.00701(9) Uani 1 4 d S T P
Fe Fe 1.0000 0.5000 0.5000 0.00752(18) Uani 1 4 d S T P
N1 N 1.0000 0.5701(6) 0.3713(3) 0.0096(8) Uani 1 2 d S T P
N2 N 0.8094(4) 0.3095(4) 0.48087(18) 0.0128(6) Uani 1 1 d . . .
N3 N 1.0000 0.6721(7) 0.1913(3) 0.0292(12) Uani 1 2 d S T P
C1 C 1.0000 0.7534(7) 0.3457(3) 0.0188(11) Uani 1 2 d S T P
H1 H 1.0000 0.8509 0.3880 0.023 Uiso 1 2 calc R U P
C2 C 1.0000 0.7961(8) 0.2560(4) 0.0251(13) Uani 1 2 d S T P
C3 C 1.0000 0.4886(8) 0.2185(4) 0.0277(13) Uani 1 2 d S T P
H3 H 1.0000 0.3931 0.1753 0.033 Uiso 1 2 calc R U P
C4 C 1.0000 0.4347(8) 0.3066(4) 0.0178(11) Uani 1 2 d S T P
H4 H 1.0000 0.3057 0.3217 0.021 Uiso 1 2 calc R U P
C5 C 0.6951(5) 0.1970(5) 0.4842(2) 0.0120(7) Uani 1 1 d . . .
F F 1.0000 0.9827(4) 0.2317(3) 0.0481(12) Uani 1 2 d S T P
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt 0.00460(13) 0.00451(12) 0.01193(13) 0.00016(11) 0.000 0.000
Fe 0.0043(4) 0.0050(4) 0.0133(5) 0.0019(4) 0.000 0.000
N1 0.005(2) 0.0121(18) 0.012(2) 0.0027(16) 0.000 0.000
N2 0.0101(14) 0.0107(13) 0.0175(16) 0.0005(11) -0.0006(11) 0.0018(13)
N3 0.039(3) 0.028(3) 0.020(3) 0.008(2) 0.000 0.000
C1 0.021(3) 0.016(3) 0.020(3) 0.002(2) 0.000 0.000
C2 0.032(3) 0.023(3) 0.021(3) 0.011(2) 0.000 0.000
C3 0.030(3) 0.026(3) 0.027(3) -0.013(3) 0.000 0.000
C4 0.018(3) 0.014(2) 0.022(3) -0.001(2) 0.000 0.000
C5 0.0110(16) 0.0077(15) 0.0174(19) 0.0013(12) -0.0007(12) 0.0015(14)
F 0.095(4) 0.023(2) 0.027(2) 0.0126(16) 0.000 0.000
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'
F F 0.0171 0.0103 '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'
Pt Pt -1.7033 8.3905 '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
C5 Pt C5 180.00(14) 5_656 .
C5 Pt C5 89.2(2) 5_656 7_655
C5 Pt C5 90.8(2) . 7_655
C5 Pt C5 90.8(2) 5_656 3_556
C5 Pt C5 89.2(2) . 3_556
C5 Pt C5 180.00(18) 7_655 3_556
N1 Fe N1 180.0 5_766 .
N2 Fe N1 88.54(12) . 5_766
N2 Fe N1 91.46(12) 5_766 5_766
N2 Fe N1 88.54(12) 7_755 5_766
N2 Fe N1 91.46(12) 3_566 5_766
N2 Fe N1 91.46(12) . .
N2 Fe N1 88.54(12) 5_766 .
N2 Fe N1 91.46(12) 7_755 .
N2 Fe N1 88.54(12) 3_566 .
N2 Fe N2 180.0 . 5_766
N2 Fe N2 90.90(17) . 7_755
N2 Fe N2 89.10(17) 5_766 7_755
N2 Fe N2 89.10(17) . 3_566
N2 Fe N2 90.90(17) 5_766 3_566
N2 Fe N2 180.0 7_755 3_566
C1 N1 C4 117.5(5) . .
C1 N1 Fe 120.9(3) . .
C4 N1 Fe 121.5(4) . .
C5 N2 Fe 169.0(3) . .
C2 N3 C3 114.1(5) . .
N1 C1 C2 119.2(5) . .
N1 C1 H1 120.4 . .
C2 C1 H1 120.4 . .
N3 C2 F 116.2(5) . .
N3 C2 C1 125.8(5) . .
F C2 C1 118.1(5) . .
N3 C3 C4 123.6(5) . .
N3 C3 H3 118.2 . .
C4 C3 H3 118.2 . .
N1 C4 C3 119.9(5) . .
N1 C4 H4 120.1 . .
C3 C4 H4 120.1 . .
N2 C5 Pt 175.6(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt C5 1.989(4) 5_656
Pt C5 1.989(4) .
Pt C5 1.989(4) 7_655
Pt C5 1.989(4) 3_556
Fe N1 1.990(4) 5_766
Fe N1 1.990(4) .
Fe N2 1.941(3) .
Fe N2 1.941(3) 5_766
Fe N2 1.941(3) 7_755
Fe N2 1.941(3) 3_566
N1 C1 1.337(6) .
N1 C4 1.355(7) .
N2 C5 1.143(5) .
N3 C2 1.300(7) .
N3 C3 1.345(7) .
C1 C2 1.378(7) .
C1 H1 0.9300 .
C2 F 1.354(6) .
C3 C4 1.373(8) .
C3 H3 0.9300 .
C4 H4 0.9300 .