#------------------------------------------------------------------------------
#$Date: 2021-04-05 16:55:09 +0200 (lun 05 de abr de 2021) $
#$Revision: 263781 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/67/7706724.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_7706724
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                 108.690(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4484(14)
_cell_length_b                   7.9306(7)
_cell_length_c                   12.8457(11)
_cell_measurement_reflns_used    4425
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.176
_cell_measurement_theta_min      2.784
_cell_volume                     1490.8(2)
_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      150(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 0.998
_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  0.0532
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_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            7123
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.213
_diffrn_reflns_theta_min         2.921
_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    10.947
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.4461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS (Krause, 2015) was used for absorption correction.
wR2(int) was 0.1177 before and 0.0663 after correction.
The Ratio of minimum to maximum transmission is 0.5984.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.822
_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         0.952
_refine_diff_density_min         -1.487
_refine_diff_density_rms         0.192
_refine_ls_extinction_coef       0.00040(8)
_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   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     80
_refine_ls_number_reflns         1671
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0303
_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)+(0.0197P)²+10.1040P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0680
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1321
_reflns_number_total             1671
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt04071a2.cif
_cod_data_source_block           Cu(2ip)2Br2_150K
_cod_depositor_comments
'Adding full bibliography for 7706719--7706724.cif.'
_cod_database_code               7706724
_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   0.560
_shelx_estimated_absorpt_t_min   0.273
_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 TCD1624 in C2/c
    tcd1624.res
    created by SHELXL-2018/3 at 08:20:32 on 16-Feb-2021
CELL 0.71073 15.4484 7.9306 12.8457 90 108.6899 90
ZERR 4 0.0014 0.0007 0.0011 0 0.003 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. 4 0 0
PLAN  2
SIZE 0.06 0.1 0.16
TEMP -123.15
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 "%.\\TCD1624.hkl">
REM </olex2.extras>

WGHT    0.019700   10.104000
EXTI    0.000398
FVAR       0.05667
I1    5    0.358020    0.807975    0.309873    11.00000    0.03451    0.02405 =
         0.02087    0.00292    0.01086   -0.00019
BR1   3    0.121493    0.646013    0.354169    11.00000    0.02494    0.02495 =
         0.01946   -0.00294    0.00387    0.00171
CU1   4    0.250000    0.750000    0.500000    10.50000    0.02214    0.01721 =
         0.01482    0.00018    0.00624    0.00293
N1    6    0.326301    0.567890    0.470956    11.00000    0.02259    0.01677 =
         0.01675    0.00104    0.00269    0.00008
C1    1    0.367387    0.578241    0.394521    11.00000    0.02328    0.02021 =
         0.01441   -0.00060    0.00375   -0.00150
C2    1    0.415163    0.444532    0.369271    11.00000    0.02849    0.02725 =
         0.01953   -0.00649    0.00862    0.00206
AFIX  43
H2    2    0.442419    0.454074    0.312913    11.00000   -1.20000
AFIX   0
C3    1    0.421808    0.297220    0.428674    11.00000    0.02899    0.01908 =
         0.03492   -0.00768    0.01126    0.00546
AFIX  43
H3    2    0.454162    0.203322    0.413751    11.00000   -1.20000
AFIX   0
C4    1    0.381299    0.287081    0.509677    11.00000    0.02277    0.02940 =
         0.03187    0.00131    0.00828    0.00476
AFIX  43
H4    2    0.385762    0.186662    0.551395    11.00000   -1.20000
AFIX   0
C5    1    0.334526    0.423624    0.529261    11.00000    0.03334    0.02260 =
         0.02259   -0.00102    0.01061    0.00388
AFIX  43
H5    2    0.307035    0.416713    0.585527    11.00000   -1.20000
AFIX   0
HKLF 4




REM  TCD1624 in C2/c
REM wR2 = 0.067970, GooF = S = 1.07069, Restrained GooF = 1.07069 for all data
REM R1 = 0.030300 for 1321 Fo > 4sig(Fo) and 0.047150 for all 1671 data
REM 80 parameters refined using 0 restraints

END

WGHT      0.0197     10.0847

REM Highest difference peak  0.952,  deepest hole -1.487,  1-sigma level  0.192
Q1    1   0.3616  0.5745  0.3134  11.00000  0.05    0.95
Q2    1   0.4609  0.8020  0.3341  11.00000  0.05    0.92
;
_shelx_res_checksum              6787
_olex2_exptl_crystal_mounting_method 'mounted in oil on a MiTeGen microloop'
_olex2_submission_original_sample_id 'Cu(2Ip)2Br 150K'
_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 0.35802(3) 0.80797(5) 0.30987(3) 0.02600(14) Uani 1 1 d . . . . .
Br1 Br 0.12149(4) 0.64601(7) 0.35417(5) 0.02389(16) Uani 1 1 d . . . . .
Cu1 Cu 0.250000 0.750000 0.500000 0.0180(2) Uani 1 2 d S . P . .
N1 N 0.3263(3) 0.5679(5) 0.4710(4) 0.0196(10) Uani 1 1 d . . . . .
C1 C 0.3674(4) 0.5782(7) 0.3945(4) 0.0198(11) Uani 1 1 d . . . . .
C2 C 0.4152(4) 0.4445(7) 0.3693(5) 0.0249(12) Uani 1 1 d . . . . .
H2 H 0.442419 0.454074 0.312913 0.030 Uiso 1 1 calc R U . . .
C3 C 0.4218(4) 0.2972(7) 0.4287(5) 0.0274(13) Uani 1 1 d . . . . .
H3 H 0.454162 0.203322 0.413751 0.033 Uiso 1 1 calc R U . . .
C4 C 0.3813(4) 0.2871(8) 0.5097(5) 0.0281(13) Uani 1 1 d . . . . .
H4 H 0.385762 0.186662 0.551395 0.034 Uiso 1 1 calc R U . . .
C5 C 0.3345(4) 0.4236(7) 0.5293(5) 0.0258(13) Uani 1 1 d . . . . .
H5 H 0.307035 0.416713 0.585527 0.031 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 0.0345(2) 0.0241(2) 0.0209(2) 0.00292(15) 0.01086(16) -0.00019(16)
Br1 0.0249(3) 0.0249(3) 0.0195(3) -0.0029(2) 0.0039(2) 0.0017(2)
Cu1 0.0221(5) 0.0172(5) 0.0148(5) 0.0002(3) 0.0062(4) 0.0029(4)
N1 0.023(2) 0.017(2) 0.017(2) 0.0010(18) 0.0027(18) 0.0001(18)
C1 0.023(3) 0.020(3) 0.014(3) -0.001(2) 0.004(2) -0.001(2)
C2 0.028(3) 0.027(3) 0.020(3) -0.006(2) 0.009(2) 0.002(2)
C3 0.029(3) 0.019(3) 0.035(3) -0.008(3) 0.011(3) 0.005(2)
C4 0.023(3) 0.029(3) 0.032(3) 0.001(3) 0.008(3) 0.005(2)
C5 0.033(3) 0.023(3) 0.023(3) -0.001(2) 0.011(3) 0.004(2)
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 90.24(13) . 7_566 ?
N1 Cu1 Br1 90.24(13) 7_566 . ?
N1 Cu1 Br1 89.76(13) 7_566 7_566 ?
N1 Cu1 Br1 89.76(13) . . ?
N1 Cu1 N1 180.0 . 7_566 ?
C1 N1 Cu1 123.3(4) . . ?
C1 N1 C5 118.6(5) . . ?
C5 N1 Cu1 118.1(4) . . ?
N1 C1 I1 117.7(4) . . ?
N1 C1 C2 122.7(5) . . ?
C2 C1 I1 119.6(4) . . ?
C1 C2 H2 121.1 . . ?
C3 C2 C1 117.9(5) . . ?
C3 C2 H2 121.1 . . ?
C2 C3 H3 120.2 . . ?
C4 C3 C2 119.7(5) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 H4 120.4 . . ?
C5 C4 C3 119.1(6) . . ?
C5 C4 H4 120.4 . . ?
N1 C5 C4 122.0(6) . . ?
N1 C5 H5 119.0 . . ?
C4 C5 H5 119.0 . . ?
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 2.103(5) . ?
Br1 Cu1 2.3973(6) . ?
Cu1 N1 1.974(5) 7_566 ?
Cu1 N1 1.974(5) . ?
N1 C1 1.332(7) . ?
N1 C5 1.351(7) . ?
C1 C2 1.388(8) . ?
C2 H2 0.9500 . ?
C2 C3 1.381(8) . ?
C3 H3 0.9500 . ?
C3 C4 1.378(8) . ?
C4 H4 0.9500 . ?
C4 C5 1.369(8) . ?
C5 H5 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 C2 C3 178.3(4) . . . . ?
Cu1 N1 C1 I1 4.9(6) . . . . ?
Cu1 N1 C1 C2 -175.0(4) . . . . ?
Cu1 N1 C5 C4 175.8(5) . . . . ?
N1 C1 C2 C3 -1.8(8) . . . . ?
C1 N1 C5 C4 -2.0(8) . . . . ?
C1 C2 C3 C4 0.2(9) . . . . ?
C2 C3 C4 C5 0.4(9) . . . . ?
C3 C4 C5 N1 0.5(9) . . . . ?
C5 N1 C1 I1 -177.4(4) . . . . ?
C5 N1 C1 C2 2.7(8) . . . . ?
