Experimental and theoretical insights for designing Zn<sup>2+</sup> complexes to trigger chemo-selective hetero-coupling of alcohols.
Samanta, Arup; Behera, Prativa; Chaubey, Amit; Mondal, Avijit; Pal, Debjyoti; Mohar, Kailash; Roy, Lisa; Srimani, Dipankar; Chemical communications (Cambridge, England) 60 (2024) 4056–4059; doi:10.1039/d4cc00864b

data_7132825
_publ_section_title
;
 Experimental and theoretical insights for designing Zn<sup>2+</sup>
 complexes to trigger chemo-selective hetero-coupling of alcohols.
;
_journal_issue                   30
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4056
_journal_page_last               4059
_journal_paper_doi               10.1039/d4cc00864b
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C12 H11 Br2 N3 Zn'
_chemical_formula_sum            'C12 H11 Br2 N3 Zn'
_chemical_formula_weight         422.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-01-16
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-01-24 deposited with the CCDC.	2024-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                77.783(10)
_cell_angle_beta                 85.879(13)
_cell_angle_gamma                77.735(11)
_cell_formula_units_Z            2
_cell_length_a                   7.8069(14)
_cell_length_b                   7.8757(8)
_cell_length_c                   11.9902(16)
_cell_measurement_reflns_used    1114
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.7070
_cell_measurement_theta_min      2.7010
_cell_volume                     703.79(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2760
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.879
_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    -70.00 -44.00   1.00   16.47    --  -17.33-178.00  90.00   26
  2  \w    -20.00  21.00   1.00   16.47    --  -17.33 -99.00 -30.00   41
  3  \w    -19.00  24.00   1.00   16.47    --  -17.33 -99.00 150.00   43
  4  \w     35.00  94.00   1.00   16.47    --   20.92-178.00   0.00   59
  5  \w     -4.00  82.00   1.00   16.47    --   20.92  38.00 150.00   86
  6  \w    -40.00  65.00   1.00   16.47    --   20.92 -19.00 -60.00  105
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0506358000
_diffrn_orient_matrix_UB_12      -0.0637217000
_diffrn_orient_matrix_UB_13      0.0253824000
_diffrn_orient_matrix_UB_21      0.0713547000
_diffrn_orient_matrix_UB_22      -0.0479406000
_diffrn_orient_matrix_UB_23      0.0346631000
_diffrn_orient_matrix_UB_31      -0.0315628000
_diffrn_orient_matrix_UB_32      0.0499507000
_diffrn_orient_matrix_UB_33      0.0426692000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0889
_diffrn_reflns_av_unetI/netI     0.1732
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5082
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.679
_diffrn_reflns_theta_min         2.671
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.407
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.23a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.993
_exptl_crystal_description       Block
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.238
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         3204
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.1565
_refine_ls_R_factor_gt           0.0817
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0735P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1732
_refine_ls_wR_factor_ref         0.2279
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1409
_reflns_number_total             3204
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00864b2.cif
_cod_data_source_block           as-ph-1
_cod_depositor_comments
'Adding full bibliography for 7132825--7132828.cif.'
_cod_database_code               7132825
_shelx_shelxl_version_number     2019/1
_chemical_oxdiff_formula         ZnNCBrH
_diffrn_oxdiff_ac4_digest_frames
;
01b4f329f3d147bbe36155cf741d32914b00027cde7
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C1-C2 = C4-C5 = C5-C6
 1.37 with sigma of 0.02
 C1-C6
 1.38 with sigma of 0.02
 C2-C3 = C3-C4
 1.36 with sigma of 0.02
 C1-C5
 2.38 with sigma of 0.04
 C2-C4
 2.36 with sigma of 0.04
 C1-C3 = C3-C5 = C4-C6
 2.37 with sigma of 0.04
 C1-C2 \\sim C2-C3 \\sim C3-C4 \\sim C4-C5 \\sim C5-C6 \\sim C6-C1
 with sigma of 0.02
 C1-C5 \\sim C1-C3 \\sim C5-C3 \\sim C4-C2 \\sim C4-C6 \\sim C6-C2
 with sigma of 0.04
3. Restrained planarity
 C1, C2, C3, C4, C5, C6
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C5, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12), C1(H1), C2(H2A), C3(H3),
  C4(H4), C5(H5)
;
_shelx_res_checksum              34490
_shelx_hkl_checksum              17911
_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 2.869
_oxdiff_exptl_absorpt_empirical_full_min 0.242