#------------------------------------------------------------------------------
#$Date: 2024-04-05 01:09:58 +0200 (Fri 05 de Apr de 2024) $
#$Revision: 290900 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/81/7248102.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_7248102
loop_
_publ_author_name
'Zaguzin, Alexander S.'
'Zaitsev, Artem V.'
'Korobeynikov, Nikita A.'
'Novikov, Alexander S.'
'Usoltsev, Andrey N.'
'Fedin, Vladimir P.'
'Adonin, Sergey A.'
_publ_section_title
;
 4,5-Diiodo-1-H-imidazole-derived linker ligand and Cu(i) and Co(ii)
 coordination polymers based thereupon
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              1607
_journal_page_last               1612
_journal_paper_doi               10.1039/D4CE00072B
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C10 H10 I4 N4'
_chemical_formula_sum            'C10 H10 I4 N4'
_chemical_formula_weight         693.82
_chemical_name_systematic        1,4-bis(4,5-diiodoimidazol-1-yl)butane
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-01
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-10 deposited with the CCDC.	2024-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7171(3)
_cell_length_b                   12.9296(5)
_cell_length_c                   14.2643(5)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      31.46
_cell_measurement_theta_min      3.15
_cell_volume                     1607.71(10)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.00
_diffrn_detector                 PIXEL
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Incoatec HELIOS multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28635
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.513
_diffrn_reflns_theta_min         3.151
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    7.743
_exptl_absorpt_correction_T_max  0.6049
_exptl_absorpt_correction_T_min  0.3980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0975 before and 0.0460 after correction.
The Ratio of minimum to maximum transmission is 0.6580.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.866
_exptl_crystal_description       plate
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         2606
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0139
_refine_ls_R_factor_gt           0.0134
_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)+(0.0072P)²+1.1732P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0311
_refine_ls_wR_factor_ref         0.0313
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2540
_reflns_number_total             2606
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00072b2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7248102--7248104.cif.'
_cod_database_code               7248102
_shelx_shelxl_version_number     2017/1
_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   0.511
_shelx_estimated_absorpt_t_min   0.353
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_shelx_res_file
;
TITL 1_a.res in Pbca
    1.res
    created by SHELXL-2017/1 at 17:01:22 on 01-Dec-2023
REM Old TITL 1 in Pbca
REM SHELXT solution in Pbca
REM R1 0.119, Rweak 0.001, Alpha 0.015, Orientation as input
REM Formula found by SHELXT: C6 N I2
CELL 0.71073 8.7171 12.9296 14.2643 90 90 90
ZERR 4 0.0003 0.0005 0.0005 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H I N
UNIT 40 40 16 16

L.S. 10 0 0
PLAN  8
SIZE 0.17 0.14 0.1
TEMP -123.15
CONF
list 4
MORE -1
BOND $H
fmap 2 53
acta
OMIT 1 1 5
OMIT 1 1 6
OMIT 1 2 7
OMIT 1 3 8
OMIT 1 5 4
OMIT 2 2 0
OMIT 3 4 1
OMIT 3 8 4
OMIT 4 3 0
REM <olex2.extras>
REM <HklSrc "%.\\1.hkl">
REM </olex2.extras>

WGHT    0.007200    1.173200
FVAR       0.25088
I1    3    0.327731    0.672676    0.273668    11.00000    0.02039    0.02361 =
         0.01910    0.00047   -0.00613    0.00200
I2    3    0.583666    0.429623    0.341267    11.00000    0.02181    0.01474 =
         0.02789   -0.00317    0.00090    0.00001
C1    1    0.502811    0.663835    0.371323    11.00000    0.01536    0.01707 =
         0.01661    0.00004   -0.00162    0.00179
N2    4    0.684915    0.610200    0.464774    11.00000    0.01376    0.01841 =
         0.01788   -0.00048   -0.00197    0.00223
N1    4    0.547215    0.748295    0.422439    11.00000    0.02146    0.01758 =
         0.02306   -0.00310   -0.00416    0.00212
C2    1    0.585174    0.577347    0.395940    11.00000    0.01466    0.01463 =
         0.01672   -0.00075    0.00069    0.00042
C4    1    0.794716    0.548409    0.519493    11.00000    0.01584    0.02498 =
         0.01890    0.00343   -0.00142    0.00445
AFIX  23
H4A   2    0.746893    0.481238    0.535486    11.00000   -1.20000
H4B   2    0.817331    0.584930    0.578907    11.00000   -1.20000
AFIX   0
C5    1    0.944368    0.528534    0.467826    11.00000    0.01444    0.02045 =
         0.01967    0.00111   -0.00168    0.00213
AFIX  23
H5A   2    0.990049    0.595076    0.447836    11.00000   -1.20000
H5B   2    0.924380    0.486494    0.411119    11.00000   -1.20000
AFIX   0
C3    1    0.657273    0.712527    0.477608    11.00000    0.02040    0.01904 =
         0.02296   -0.00390   -0.00361   -0.00010
AFIX  43
H3    2    0.711190    0.754104    0.521535    11.00000   -1.20000
AFIX   0
HKLF 4




REM  1_a.res in Pbca
REM R1 =  0.0134 for    2540 Fo > 4sig(Fo)  and  0.0139 for all    2606 data
REM     82 parameters refined using      0 restraints

END

WGHT      0.0074      1.1676

REM Highest difference peak  0.474,  deepest hole -0.479,  1-sigma level  0.081
Q1    1   0.3972  0.6617  0.2360  11.00000  0.05    0.47
Q2    1   0.5330  0.4212  0.3005  11.00000  0.05    0.40
Q3    1   0.7173  0.7470  0.5852  11.00000  0.05    0.39
Q4    1   0.6543  0.5942  0.4243  11.00000  0.05    0.39
Q5    1   0.8720  0.5400  0.4965  11.00000  0.05    0.38
Q6    1   0.5431  0.6192  0.3795  11.00000  0.05    0.37
Q7    1   0.6834  0.6601  0.4678  11.00000  0.05    0.37
Q8    1   0.3225  0.6209  0.2809  11.00000  0.05    0.35
;
_shelx_res_checksum              43209
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
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
I1 I 0.32773(2) 0.67268(2) 0.27367(2) 0.02103(3) Uani 1 1 d . . . . .
I2 I 0.58367(2) 0.42962(2) 0.34127(2) 0.02148(3) Uani 1 1 d . . . . .
C1 C 0.50281(17) 0.66383(11) 0.37132(10) 0.0163(3) Uani 1 1 d . . . . .
N2 N 0.68492(14) 0.61020(10) 0.46477(9) 0.0167(2) Uani 1 1 d . . . . .
N1 N 0.54722(16) 0.74830(10) 0.42244(9) 0.0207(2) Uani 1 1 d . . . . .
C2 C 0.58517(16) 0.57735(11) 0.39594(10) 0.0153(2) Uani 1 1 d . . . . .
C4 C 0.79472(17) 0.54841(13) 0.51949(11) 0.0199(3) Uani 1 1 d . . . . .
H4A H 0.746893 0.481238 0.535486 0.024 Uiso 1 1 calc R U . . .
H4B H 0.817331 0.584930 0.578907 0.024 Uiso 1 1 calc R U . . .
C5 C 0.94437(16) 0.52853(12) 0.46783(10) 0.0182(3) Uani 1 1 d . . . . .
H5A H 0.990049 0.595076 0.447836 0.022 Uiso 1 1 calc R U . . .
H5B H 0.924380 0.486494 0.411119 0.022 Uiso 1 1 calc R U . . .
C3 C 0.65727(18) 0.71253(12) 0.47761(11) 0.0208(3) Uani 1 1 d . . . . .
H3 H 0.711190 0.754104 0.521535 0.025 Uiso 1 1 calc R U . . .
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
I1 0.02039(5) 0.02361(5) 0.01910(5) 0.00047(3) -0.00613(3) 0.00200(3)
I2 0.02181(5) 0.01474(5) 0.02789(6) -0.00317(3) 0.00090(4) 0.00001(3)
C1 0.0154(6) 0.0171(6) 0.0166(6) 0.0000(5) -0.0016(5) 0.0018(5)
N2 0.0138(5) 0.0184(6) 0.0179(5) -0.0005(4) -0.0020(4) 0.0022(4)
N1 0.0215(6) 0.0176(6) 0.0231(6) -0.0031(5) -0.0042(5) 0.0021(5)
C2 0.0147(6) 0.0146(6) 0.0167(6) -0.0007(5) 0.0007(5) 0.0004(5)
C4 0.0158(6) 0.0250(7) 0.0189(6) 0.0034(6) -0.0014(5) 0.0044(5)
C5 0.0144(6) 0.0204(7) 0.0197(6) 0.0011(5) -0.0017(5) 0.0021(5)
C3 0.0204(7) 0.0190(7) 0.0230(7) -0.0039(5) -0.0036(5) -0.0001(5)
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'
I I -0.4742 1.8119 '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'
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
N1 C1 I1 121.53(10) . . ?
N1 C1 C2 111.42(13) . . ?
C2 C1 I1 127.02(11) . . ?
C2 N2 C4 128.39(13) . . ?
C3 N2 C2 106.53(12) . . ?
C3 N2 C4 124.99(13) . . ?
C3 N1 C1 104.05(13) . . ?
C1 C2 I2 130.79(11) . . ?
C1 C2 N2 105.11(12) . . ?
N2 C2 I2 123.95(10) . . ?
N2 C4 H4A 109.0 . . ?
N2 C4 H4B 109.0 . . ?
N2 C4 C5 113.14(12) . . ?
H4A C4 H4B 107.8 . . ?
C5 C4 H4A 109.0 . . ?
C5 C4 H4B 109.0 . . ?
C4 C5 C5 109.61(15) . 5_766 ?
C4 C5 H5A 109.7 . . ?
C4 C5 H5B 109.7 . . ?
C5 C5 H5A 109.7 5_766 . ?
C5 C5 H5B 109.7 5_766 . ?
H5A C5 H5B 108.2 . . ?
N2 C3 H3 123.6 . . ?
N1 C3 N2 112.89(13) . . ?
N1 C3 H3 123.6 . . ?
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
I1 C1 2.0695(14) . ?
I2 C2 2.0631(14) . ?
C1 N1 1.3689(19) . ?
C1 C2 1.3745(19) . ?
N2 C2 1.3786(18) . ?
N2 C4 1.4709(19) . ?
N2 C3 1.357(2) . ?
N1 C3 1.324(2) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.520(2) . ?
C5 C5 1.526(3) 5_766 ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C3 H3 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
I1 C1 N1 C3 178.66(11) . . . . ?
I1 C1 C2 I2 5.8(2) . . . . ?
I1 C1 C2 N2 -178.51(10) . . . . ?
C1 N1 C3 N2 -0.25(18) . . . . ?
N2 C4 C5 C5 175.64(15) . . . 5_766 ?
N1 C1 C2 I2 -175.96(11) . . . . ?
N1 C1 C2 N2 -0.30(17) . . . . ?
C2 C1 N1 C3 0.34(18) . . . . ?
C2 N2 C4 C5 82.01(19) . . . . ?
C2 N2 C3 N1 0.07(18) . . . . ?
C4 N2 C2 I2 -7.3(2) . . . . ?
C4 N2 C2 C1 176.67(14) . . . . ?
C4 N2 C3 N1 -176.61(14) . . . . ?
C3 N2 C2 I2 176.17(11) . . . . ?
C3 N2 C2 C1 0.13(16) . . . . ?
C3 N2 C4 C5 -102.04(17) . . . . ?
