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_7245843
_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_absolute_configuration ad
_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             2019-11-13
_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.	2022-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.285(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1101(2)
_cell_length_b                   10.85749(19)
_cell_length_c                   13.0218(3)
_cell_measurement_reflns_used    13456
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      30.0140
_cell_measurement_theta_min      3.0230
_cell_volume                     1364.85(5)
_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 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -14.00  83.00   0.50    6.00    --    3.35  38.00   0.00  194
  2  \w    -22.00  78.00   0.50    6.00    --    3.35  77.00  90.00  200
  3  \w    -27.00  31.00   0.50    6.00    --   -4.60 -99.00 150.00  116
  4  \w    -27.00  26.00   0.50    6.00    --    3.35 -99.00 -30.00  106
  5  \w    -77.00   5.00   0.50    6.00    --    3.35 -19.00  30.00  164
  6  \w    -22.00  69.00   0.50    6.00    --   -4.60  57.00-180.00  182
  7  \w    -50.00 -23.00   0.50    6.00    --   -4.60 115.00   3.85   54
  8  \w    -52.00 -26.00   0.50    6.00    --   -4.60 119.00-116.49   52
  9  \w    -86.00  76.00   0.50    6.00    --   -4.60   0.00-180.00  324
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0147922000
_diffrn_orient_matrix_UB_12      -0.0446251000
_diffrn_orient_matrix_UB_13      -0.0416599000
_diffrn_orient_matrix_UB_21      -0.0612948000
_diffrn_orient_matrix_UB_22      0.0323594000
_diffrn_orient_matrix_UB_23      -0.0273487000
_diffrn_orient_matrix_UB_31      0.0377035000
_diffrn_orient_matrix_UB_32      0.0350625000
_diffrn_orient_matrix_UB_33      -0.0277747000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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            14452
_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         26.367
_diffrn_reflns_theta_min         2.490
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.867
_exptl_absorpt_correction_T_max  0.771
_exptl_absorpt_correction_T_min  0.530
_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    1.786
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.155
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Flack x determined using 1277 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2797
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0134
_refine_ls_R_factor_gt           0.0131
_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^)+(0.0200P)^2^+0.5222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0334
_refine_ls_wR_factor_ref         0.0335
_reflns_Friedel_coverage         0.894
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                2758
_reflns_number_total             2797
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01311h2.cif
_cod_data_source_block           hadi1411
_cod_depositor_comments
'Adding full bibliography for 7245842--7245847.cif.'
_cod_original_cell_volume        1364.86(5)
_cod_database_code               7245843
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.747
_shelx_estimated_absorpt_t_min   0.433
_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              93681
_shelx_hkl_checksum              40302