Pseudotetrahedral Zn(II)-(R or S)-dihalogen-salicylaldiminato complexes with Λ- or Δ-chirality induction at-metal
Amiri Rudbari, Hadi; Saadati, Arezoo; Ariaeefar, Mahnaz; Blacque, Olivier; Correia, Isabel; Islam, Mohammad Khairul; Woschko, Dennis; Janiak, Christoph; Enamullah, Mohammed; Dalton Transactions  (2022) –; doi:10.1039/D1DT04220C

data_7709193
_publ_section_title
;
 Pseudotetrahedral Zn(II)-(R or S)-dihalogen-salicylaldiminato complexes
 with \L- or \D-chirality induction at-metal
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04220C
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C30 H24 Br2 Cl2 N2 O2 Zn'
_chemical_formula_sum            'C30 H24 Br2 Cl2 N2 O2 Zn'
_chemical_formula_weight         740.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-02 deposited with the CCDC.	2021-12-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.216(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2247(2)
_cell_length_b                   10.8940(3)
_cell_length_c                   12.9214(3)
_cell_measurement_reflns_used    6125
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      76.1140
_cell_measurement_theta_min      4.8590
_cell_volume                     1374.80(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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   -114.00 -13.00   1.00    1.00    --  -41.44 -57.00   0.00  101
  2  \w    -82.00  39.00   1.00    1.00    --  -41.44  19.00 -30.00  121
  3  \w    -70.00  32.00   1.00    1.00    --  -41.44  57.00-180.00  102
  4  \w     23.00  97.00   1.00    1.00    --   41.44-125.00 -60.00   74
  5  \w     23.00  97.00   1.00    1.00    --   41.44-125.00  60.00   74
  6  \w     17.00 116.00   1.00    1.00    --   41.44  37.00  30.00   99
  7  \w      1.00  82.00   1.00    1.00    --   41.44 -99.00 -30.00   81
  8  \w    100.00 178.00   1.00    3.00    --  112.00 111.00  60.00   78
  9  \w     39.00 138.00   1.00    3.00    --  112.00 -45.00 120.00   99
 10  \w     59.00 178.00   1.00    3.00    --  112.00  15.00  60.00  119
 11  \w     29.00 110.00   1.00    3.00    --  112.00 -94.00 -30.00   81
 12  \w     59.00 178.00   1.00    3.00    --  112.00  15.00 -60.00  119
 13  \w     36.00 113.00   1.00    3.00    --  112.00-111.00 -60.00   77
 14  \w     86.00 178.00   1.00    3.00    --  112.00  45.00-150.00   92
 15  \w     86.00 178.00   1.00    3.00    --  112.00  45.00  90.00   92
 16  \w     29.00 110.00   1.00    3.00    --  112.00 -94.00-150.00   81
 17  \w     84.00 178.00   1.00    3.00    --  112.00  30.00 -30.00   94
 18  \w     79.00 178.00   1.00    3.00    --  112.00  77.00   0.00   99
 19  \w     39.00 138.00   1.00    3.00    --  112.00 -45.00  30.00   99
 20  \w     83.00 178.00   1.00    3.00    --  112.00  61.00  60.00   95
 21  \w     36.00 113.00   1.00    3.00    --  112.00-111.00-150.00   77
 22  \w     36.00 113.00   1.00    3.00    --  112.00-111.00 -90.00   77
 23  \w     84.00 178.00   1.00    3.00    --  112.00  30.00 150.00   94
 24  \w     79.00 178.00   1.00    3.00    --  112.00  77.00 -30.00   99
 25  \w     86.00 178.00   1.00    3.00    --  112.00  45.00  60.00   92
 26  \w     84.00 178.00   1.00    3.00    --  112.00  30.00  60.00   94
 27  \w     36.00 140.00   1.00    3.00    --  112.00 -30.00 -90.00  104
 28  \w     79.00 153.00   1.00    3.00    --  112.00  77.00  30.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1161669000
_diffrn_orient_matrix_UB_12      -0.0525164000
_diffrn_orient_matrix_UB_13      -0.0402140000
_diffrn_orient_matrix_UB_21      0.0341028000
_diffrn_orient_matrix_UB_22      -0.0937495000
_diffrn_orient_matrix_UB_23      0.0935349000
_diffrn_orient_matrix_UB_31      -0.1011876000
_diffrn_orient_matrix_UB_32      -0.0917049000
_diffrn_orient_matrix_UB_33      -0.0723943000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0154
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8416
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.427
_diffrn_reflns_theta_min         4.872
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.697
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.452
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_description       plate
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.190
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 1258 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2762
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0222
_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^)+(0.0409P)^2^+0.9935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0589
_reflns_Friedel_coverage         0.869
_reflns_Friedel_fraction_full    0.979
_reflns_Friedel_fraction_max     0.965
_reflns_number_gt                2732
_reflns_number_total             2762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04220c2.cif
_cod_data_source_block           hadi2011
_cod_database_code               7709193
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_usercomment     'sample S'
_shelx_estimated_absorpt_t_max   0.824
_shelx_estimated_absorpt_t_min   0.348
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C8(H8)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
;
_shelx_res_checksum              77980
_shelx_hkl_checksum              78493