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_7709192
_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 Br4 N2 O2 Zn'
_chemical_formula_sum            'C30 H24 Br4 N2 O2 Zn'
_chemical_formula_weight         829.52
_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             2019-11-18
_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                 106.622(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2155(3)
_cell_length_b                   10.9297(3)
_cell_length_c                   12.9935(3)
_cell_measurement_reflns_used    13802
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      29.9690
_cell_measurement_theta_min      2.9630
_cell_volume                     1390.13(7)
_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    -15.00  77.00   0.50    8.00    --    3.35  57.00 -60.00  184
  2  \w     38.00  84.00   0.50    8.00    --    3.35 178.00 120.00   92
  3  \w    -44.00 -14.00   0.50    8.00    --   -4.60 105.00-139.58   60
  4  \w    -44.00 -15.00   0.50    8.00    --   -4.60 106.00  -9.07   58
  5  \w    -50.00 -24.00   0.50    8.00    --   -4.60 116.00 106.92   52
  6  \w    -77.00   5.00   0.50    8.00    --    3.35 -19.00 150.00  164
  7  \w    -27.00  39.00   0.50    8.00    --    3.35 -99.00 150.00  132
  8  \w    -27.00  31.00   0.50    8.00    --   -4.60 -99.00 120.00  116
  9  \w    -27.00  31.00   0.50    8.00    --   -4.60 -99.00 -30.00  116
 10  \w    -77.00  40.00   0.50    8.00    --    3.35  -3.00-132.30  234
 11  \w    -75.00  21.00   0.50    8.00    --    3.35 -38.00 -30.00  192
;
_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      -0.0615214000
_diffrn_orient_matrix_UB_12      0.0295872000
_diffrn_orient_matrix_UB_13      -0.0283379000
_diffrn_orient_matrix_UB_21      0.0339096000
_diffrn_orient_matrix_UB_22      0.0573679000
_diffrn_orient_matrix_UB_23      0.0087837000
_diffrn_orient_matrix_UB_31      0.0176903000
_diffrn_orient_matrix_UB_32      -0.0069202000
_diffrn_orient_matrix_UB_33      -0.0486331000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_unetI/netI     0.0136
_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       -15
_diffrn_reflns_number            14589
_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         2.480
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.665
_exptl_absorpt_correction_T_max  0.606
_exptl_absorpt_correction_T_min  0.379
_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    1.982
_exptl_crystal_description       prism
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 1295 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2841
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0138
_refine_ls_R_factor_gt           0.0134
_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^)+(0.0217P)^2^+0.4120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0330
_refine_ls_wR_factor_ref         0.0332
_reflns_Friedel_coverage         0.894
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                2800
_reflns_number_total             2841
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04220c2.cif
_cod_data_source_block           hadi1611
_cod_original_cell_volume        1390.14(7)
_cod_database_code               7709192
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_usercomment     (R)+Br2+Zn
_shelx_estimated_absorpt_t_max   0.618
_shelx_estimated_absorpt_t_min   0.287
_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              17594
_shelx_hkl_checksum              94788