Experimental and computational studies on pseudotetrahedral nickel(ii)-(S or R)-dihalogen-salicylaldiminates with Δ- or Λ-chirality induction at-metal
Saadati, Arezoo; Amiri Rudbari, Hadi; Aryaeifar, Mahnaz; Blacque, Olivier; Correia, Isabel; Islam, Mohammad Khairul; Woschko, Dennis; Haj Hassani Sohi, Takin; Janiak, Christoph; Enamullah, Mohammed; CrystEngComm 25 (2023) 365–377; doi:10.1039/D2CE01311H

data_7245845
_publ_section_title
;
 Experimental and computational studies on pseudotetrahedral nickel(ii)-(S
 or R)-dihalogen-salicylaldiminates with \D- or \L-chirality induction
 at-metal
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              365
_journal_page_last               377
_journal_paper_doi               10.1039/D2CE01311H
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C30 H24 Br2 Cl2 N2 Ni O2'
_chemical_formula_sum            'C30 H24 Br2 Cl2 N2 Ni O2'
_chemical_formula_weight         733.94
_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             2022-01-31
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-02-02 deposited with the CCDC.	2022-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.314(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.0967(1)
_cell_length_b                   10.8500(1)
_cell_length_c                   13.0172(2)
_cell_measurement_reflns_used    14982
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      32.6350
_cell_measurement_theta_min      2.4790
_cell_volume                     1361.41(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -70.00 109.00   1.00    6.50    --   19.62   0.00  60.00  179
  2  \w   -110.00 -61.00   1.00    6.50    --  -20.24-178.00  90.00   49
  3  \w   -110.00 -61.00   1.00    6.50    --  -20.24-178.00   0.00   49
  4  \w    -47.00  56.00   1.00    6.50    --  -20.24  37.00 -60.00  103
  5  \w    -42.00  13.00   1.00    6.50    --  -20.24 -77.00 120.00   55
  6  \w    -42.00  13.00   1.00    6.50    --  -20.24 -77.00   0.00   55
  7  \w    -42.00  13.00   1.00    6.50    --  -20.24 -77.00-180.00   55
  8  \w    -42.00  13.00   1.00    6.50    --  -20.24 -77.00 -90.00   55
  9  \w    -42.00  13.00   1.00    6.50    --  -20.24 -77.00  60.00   55
 10  \w   -109.00 -58.00   1.00    6.50    --  -20.24 178.00-120.00   51
 11  \w    -47.00  56.00   1.00    6.50    --  -20.24  37.00  30.00  103
 12  \w    -15.00  19.00   1.00    6.50    --   19.62 -99.00  30.00   34
 13  \w    -15.00  62.00   1.00    6.50    --   19.62 -99.00-180.00   77
 14  \w    -94.00   9.00   1.00    6.50    --  -20.24 -57.00  60.00  103
 15  \w   -109.00 -58.00   1.00    6.50    --  -20.24 178.00-180.00   51
 16  \w    -54.00  21.00   1.00    6.50    --  -20.24  77.00  60.00   75
;
_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      -0.0625618000
_diffrn_orient_matrix_UB_12      -0.0147474000
_diffrn_orient_matrix_UB_13      0.0114709000
_diffrn_orient_matrix_UB_21      -0.0139887000
_diffrn_orient_matrix_UB_22      -0.0465091000
_diffrn_orient_matrix_UB_23      -0.0401061000
_diffrn_orient_matrix_UB_31      0.0361162000
_diffrn_orient_matrix_UB_32      -0.0435381000
_diffrn_orient_matrix_UB_33      0.0389367000
_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  0.0272
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_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            17509
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         2.256
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.877
_exptl_absorpt_correction_T_max  0.645
_exptl_absorpt_correction_T_min  0.544
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
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            orange
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_description       cube
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.177
_refine_diff_density_min         -0.162
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 1270 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.006(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2792
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0141
_refine_ls_R_factor_gt           0.0136
_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^)+(0.0142P)^2^+0.6728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0325
_refine_ls_wR_factor_ref         0.0327
_reflns_Friedel_coverage         0.895
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2755
_reflns_number_total             2792
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01311h2.cif
_cod_data_source_block           hadi3101
_cod_depositor_comments
'Adding full bibliography for 7245842--7245847.cif.'
_cod_database_code               7245845
_shelx_estimated_absorpt_t_max   0.594
_shelx_estimated_absorpt_t_min   0.469
_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              59658
_shelx_hkl_checksum              92309