Halogen bond and polymorphism in trans-bis(2-iodo-5-halopyridine)dihalocopper(ii) complexes: crystallographic, theoretical and magnetic studies
Awwadi, Firas F.; Alwahsh, Manal I.; Turnbull, Mark M.; Landee, Christopher P.; CrystEngComm 25 (2023) 2390–2403; doi:10.1039/D2CE01711C

data_7246481
_publ_section_title
;
 Halogen bond and polymorphism in
 trans-bis(2-iodo-5-halopyridine)dihalocopper(ii) complexes:
 crystallographic, theoretical and magnetic studies
;
_journal_issue                   16
_journal_name_full               CrystEngComm
_journal_page_first              2390
_journal_page_last               2403
_journal_paper_doi               10.1039/D2CE01711C
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C10 H6 Br2 Cl2 Cu I2 N2'
_chemical_formula_sum            'C10 H6 Br2 Cl2 Cu I2 N2'
_chemical_formula_weight         702.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-12-06 deposited with the CCDC.	2023-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 128.800(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.8035(8)
_cell_length_b                   14.9629(5)
_cell_length_c                   6.6080(5)
_cell_measurement_reflns_used    1654
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.1460
_cell_measurement_theta_min      4.1000
_cell_volume                     832.48(16)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0534
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -37.00  50.00   1.00    6.00    --  -15.13  77.00 -90.00   87
  2  \w     -4.00  82.00   1.00    6.00    --   15.76  77.00  30.00   86
  3  \w     40.00  73.00   1.00    6.00    --   15.76  77.00 150.00   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0271053000
_diffrn_orient_matrix_UB_12      -0.0442595000
_diffrn_orient_matrix_UB_13      -0.0106696000
_diffrn_orient_matrix_UB_21      -0.0192865000
_diffrn_orient_matrix_UB_22      0.0113726000
_diffrn_orient_matrix_UB_23      0.0815323000
_diffrn_orient_matrix_UB_31      -0.0773623000
_diffrn_orient_matrix_UB_32      0.0126485000
_diffrn_orient_matrix_UB_33      -0.1104470000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.847
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3956
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.847
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.295
_diffrn_reflns_theta_min         3.083
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.127
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.801
_exptl_crystal_description       fragment
_exptl_crystal_F_000             638
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.629
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         1933
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0384
_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/[\s^2^(Fo^2^)+(0.0278P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0821
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1501
_reflns_number_total             1933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01711c2.cif
_cod_data_source_block           exp_1502
_cod_depositor_comments
'Adding full bibliography for 7246477--7246481.cif.'
_cod_original_cell_volume        832.48(14)
_cod_database_code               7246481
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cu Cl Br C H N'
_chemical_oxdiff_usercomment     '2c5bp cucl2 1:1 dr firas acn hot'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C4(H4), C3(H3)
;
_shelx_res_checksum              30741
_shelx_hkl_checksum              35878
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.339
_oxdiff_exptl_absorpt_empirical_full_min 0.800