#------------------------------------------------------------------------------
#$Date: 2021-04-05 17:55:09 +0300 (Mon, 05 Apr 2021) $
#$Revision: 263781 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/67/7706723.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_7706723
loop_
_publ_author_name
'Awwadi, Firas F.'
'Alwahsh, Manal I.'
'Turnbull, Mark M.'
'Landee, Christopher P.'
'Twamley, Brendan'
_publ_section_title
;
 Two new canted antiferromagnetic systems: magnetic, theoretical, and
 crystallographic studies on trans-bis(2-iodopyridine)dihalocopper(ii).
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4167
_journal_page_last               4178
_journal_paper_doi               10.1039/d0dt04071a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C10 H8 Br2 Cu I2 N2'
_chemical_formula_sum            'C10 H8 Br2 Cu I2 N2'
_chemical_formula_weight         633.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-02-16 deposited with the CCDC.	2021-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.214(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5405(17)
_cell_length_b                   7.9511(9)
_cell_length_c                   12.9193(14)
_cell_measurement_reflns_used    3161
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.951
_cell_measurement_theta_min      2.760
_cell_volume                     1516.4(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX 3 (Bruker, 2017) '
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL  (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'CMOS area detector'
_diffrn_detector_area_resol_mean 5.12
_diffrn_detector_type            'Bruker PHOTON 50'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest ECO'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_collimation    '0.5 mm double-pinhole'
_diffrn_radiation_detector       'Bruker PHOTON 50'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9674
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.130
_diffrn_reflns_theta_min         2.910
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           20.0
_diffrn_source_power             1.0
_diffrn_source_type              'Siemens, KFF Mo 2K -90 C'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    10.762
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.4778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause, 2015) was used for absorption correction.
wR2(int) was 0.1246 before and 0.0669 after correction.
The Ratio of minimum to maximum transmission is 0.6409.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.774
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.782
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.164
_refine_ls_extinction_coef       0.00049(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     80
_refine_ls_number_reflns         1681
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+18.8779P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0756
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1160
_reflns_number_total             1681
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt04071a2.cif
_cod_data_source_block           Cu(2ip)2Br2_RT
_cod_depositor_comments
'Adding full bibliography for 7706719--7706724.cif.'
_cod_database_code               7706723
_shelx_shelxl_version_number     2018/3
_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   0.564
_shelx_estimated_absorpt_t_min   0.278
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5)
;
_shelx_res_file
;
TITL TCD1625 in C2/c
    tcd1625.res
    created by SHELXL-2018/3 at 08:16:14 on 16-Feb-2021
CELL 0.71073 15.5405 7.9511 12.9193 90 108.2144 90
ZERR 4 0.0017 0.0009 0.0014 0 0.0037 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H Br Cu I N
UNIT 40 32 8 4 8 8
EQIV $1 -X,+Y,0.5-Z
EQIV $2 0.5-X,-0.5+Y,0.5-Z
EQIV $3 0.5-X,0.5+Y,0.5-Z

L.S. 14 0 0
PLAN  4
SIZE 0.06 0.1 0.16
TEMP 23(2)
CONF
RTAB Br1a Br1 Br1_$1
RTAB Br1b Br1 I1_$2
RTAB IBr1 I1 Br1_$3
BOND $H
list 4
MORE -1
fmap 2 53
acta
OMIT 2 0 0
REM <olex2.extras>
REM <HklSrc "%.\\TCD1625.hkl">
REM </olex2.extras>

WGHT    0.000000   18.877899
EXTI    0.000485
FVAR       0.05972
I1    5    0.357417    0.807360    0.309896    11.00000    0.06788    0.04856 =
         0.04211    0.00656    0.02330   -0.00055
BR1   3    0.122540    0.645806    0.356848    11.00000    0.04787    0.04826 =
         0.03950   -0.00681    0.00840    0.00379
CU1   4    0.250000    0.750000    0.500000    10.50000    0.04154    0.03272 =
         0.02926   -0.00011    0.01279    0.00548
N1    6    0.326112    0.569083    0.470789    11.00000    0.03892    0.03487 =
         0.03104    0.00223    0.01177    0.00099
C1    1    0.366644    0.579235    0.393839    11.00000    0.04764    0.03416 =
         0.03280   -0.00322    0.01186    0.00141
C2    1    0.414637    0.448135    0.369953    11.00000    0.05220    0.05093 =
         0.04821   -0.00935    0.02149    0.00774
AFIX  43
H2    2    0.442546    0.458894    0.316251    11.00000   -1.20000
AFIX   0
C3    1    0.420539    0.301175    0.426892    11.00000    0.05624    0.03741 =
         0.06576   -0.01617    0.02321    0.00543
AFIX  43
H3    2    0.451346    0.209413    0.411027    11.00000   -1.20000
AFIX   0
C4    1    0.380253    0.290199    0.508354    11.00000    0.05040    0.03741 =
         0.06104    0.00402    0.01412    0.00476
AFIX  43
H4    2    0.384753    0.192287    0.549088    11.00000   -1.20000
AFIX   0
C5    1    0.334057    0.425452    0.527450    11.00000    0.05356    0.03610 =
         0.04538    0.00148    0.02045    0.00512
AFIX  43
H5    2    0.306842    0.418212    0.581987    11.00000   -1.20000
AFIX   0
HKLF 4




REM  TCD1625 in C2/c
REM wR2 = 0.075594, GooF = S = 1.02407, Restrained GooF = 1.02407 for all data
REM R1 = 0.035261 for 1160 Fo > 4sig(Fo) and 0.065565 for all 1681 data
REM 80 parameters refined using 0 restraints

END

WGHT      0.0000     18.8651

REM Highest difference peak  0.782,  deepest hole -0.837,  1-sigma level  0.164
Q1    1   0.1259  0.7351  0.3541  11.00000  0.05    0.78
Q2    1   0.3223  0.7979  0.2867  11.00000  0.05    0.73
Q3    1   0.1220  0.8582  0.3761  11.00000  0.05    0.69
Q4    1   0.4056  0.2063  0.4731  11.00000  0.05    0.65
;
_shelx_res_checksum              66628
_olex2_exptl_crystal_mounting_method 'mounted in oil on a MiTeGen microloop'
_olex2_submission_original_sample_id 'Cu(2Ip)2Br2 RT'
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
I1 I 0.35742(4) 0.80736(7) 0.30990(4) 0.05144(19) Uani 1 1 d . . . . .
Br1 Br 0.12254(5) 0.64581(9) 0.35685(6) 0.0464(2) Uani 1 1 d . . . . .
Cu1 Cu 0.250000 0.750000 0.500000 0.0341(3) Uani 1 2 d S . P . .
N1 N 0.3261(4) 0.5691(7) 0.4708(4) 0.0348(12) Uani 1 1 d . . . . .
C1 C 0.3666(5) 0.5792(8) 0.3938(5) 0.0384(15) Uani 1 1 d . . . . .
C2 C 0.4146(5) 0.4481(9) 0.3700(6) 0.0491(19) Uani 1 1 d . . . . .
H2 H 0.442546 0.458894 0.316251 0.059 Uiso 1 1 calc R U . . .
C3 C 0.4205(5) 0.3012(9) 0.4269(6) 0.052(2) Uani 1 1 d . . . . .
H3 H 0.451346 0.209413 0.411027 0.063 Uiso 1 1 calc R U . . .
C4 C 0.3803(5) 0.2902(9) 0.5084(6) 0.0504(19) Uani 1 1 d . . . . .
H4 H 0.384753 0.192287 0.549088 0.060 Uiso 1 1 calc R U . . .
C5 C 0.3341(5) 0.4255(8) 0.5275(6) 0.0439(17) Uani 1 1 d . . . . .
H5 H 0.306842 0.418212 0.581987 0.053 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 0.0679(4) 0.0486(3) 0.0421(3) 0.0066(2) 0.0233(2) -0.0005(2)
Br1 0.0479(4) 0.0483(4) 0.0395(4) -0.0068(3) 0.0084(3) 0.0038(3)
Cu1 0.0415(7) 0.0327(6) 0.0293(6) -0.0001(5) 0.0128(5) 0.0055(5)
N1 0.039(3) 0.035(3) 0.031(3) 0.002(2) 0.012(2) 0.001(2)
C1 0.048(4) 0.034(4) 0.033(4) -0.003(3) 0.012(3) 0.001(3)
C2 0.052(5) 0.051(5) 0.048(4) -0.009(4) 0.021(4) 0.008(4)
C3 0.056(5) 0.037(4) 0.066(5) -0.016(4) 0.023(4) 0.005(4)
C4 0.050(5) 0.037(4) 0.061(5) 0.004(4) 0.014(4) 0.005(3)
C5 0.054(4) 0.036(4) 0.045(4) 0.001(3) 0.020(4) 0.005(3)
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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
Br1 Cu1 Br1 180.0 7_566 . ?
N1 Cu1 Br1 89.96(15) . 7_566 ?
N1 Cu1 Br1 89.96(15) 7_566 . ?
N1 Cu1 Br1 90.04(15) 7_566 7_566 ?
N1 Cu1 Br1 90.04(15) . . ?
N1 Cu1 N1 180.0 . 7_566 ?
C1 N1 Cu1 123.3(4) . . ?
C1 N1 C5 118.3(6) . . ?
C5 N1 Cu1 118.4(4) . . ?
N1 C1 I1 117.8(5) . . ?
N1 C1 C2 122.5(7) . . ?
C2 C1 I1 119.7(5) . . ?
C1 C2 H2 120.7 . . ?
C3 C2 C1 118.5(7) . . ?
C3 C2 H2 120.7 . . ?
C2 C3 H3 120.3 . . ?
C2 C3 C4 119.5(7) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 H4 120.7 . . ?
C5 C4 C3 118.6(7) . . ?
C5 C4 H4 120.7 . . ?
N1 C5 C4 122.6(7) . . ?
N1 C5 H5 118.7 . . ?
C4 C5 H5 118.7 . . ?
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 2.095(7) . ?
Br1 Cu1 2.3959(7) . ?
Cu1 N1 1.972(5) 7_566 ?
Cu1 N1 1.972(5) . ?
N1 C1 1.335(8) . ?
N1 C5 1.341(8) . ?
C1 C2 1.372(9) . ?
C2 H2 0.9300 . ?
C2 C3 1.368(11) . ?
C3 H3 0.9300 . ?
C3 C4 1.385(10) . ?
C4 H4 0.9300 . ?
C4 C5 1.358(10) . ?
C5 H5 0.9300 . ?
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 C2 C3 179.2(5) . . . . ?
Cu1 N1 C1 I1 5.4(7) . . . . ?
Cu1 N1 C1 C2 -175.8(5) . . . . ?
Cu1 N1 C5 C4 175.8(6) . . . . ?
N1 C1 C2 C3 0.4(11) . . . . ?
C1 N1 C5 C4 -1.1(10) . . . . ?
C1 C2 C3 C4 -1.7(11) . . . . ?
C2 C3 C4 C5 1.5(11) . . . . ?
C3 C4 C5 N1 -0.2(11) . . . . ?
C5 N1 C1 I1 -177.9(5) . . . . ?
C5 N1 C1 C2 0.9(10) . . . . ?
