Solid-state to solution helicity inversion of pseudotetrahedral chiral copper(ii) complexes with 2,4-dihalo-salicylaldiminate ligands.
Kordestani, Nazanin; Amiri Rudbari, Hadi; Bruno, Giuseppe; Rosario, Scopelliti; Braun, Jason D.; Herbert, David E.; Blacque, Olivier; Correia, Isabel; Zaman, Mohammad Al-Moktadir; Bindu, Mortuza Mamun; Janiak, Christoph; Enamullah, Mohammed; Dalton transactions (Cambridge, England : 2003) 49 (2020) 8247–8264; doi:10.1039/d0dt01649g

data_7704568
_publ_section_title
;
 Solid-state to solution helicity inversion of pseudotetrahedral chiral
 copper(ii) complexes with 2,4-dihalo-salicylaldiminate ligands.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8247
_journal_page_last               8264
_journal_paper_doi               10.1039/d0dt01649g
_journal_volume                  49
_journal_year                    2020
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C30 H24 Br2 Cl2 Cu N2 O2'
_chemical_formula_sum            'C30 H24 Br2 Cl2 Cu N2 O2'
_chemical_formula_weight         738.77
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-07-26 deposited with the CCDC.	2020-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.5551(17)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.33616(17)
_cell_length_b                   10.64041(15)
_cell_length_c                   13.0212(2)
_cell_measurement_reflns_used    3897
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      75.9990
_cell_measurement_theta_min      4.8120
_cell_volume                     1365.39(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Mercury 4.1.0 (CCDC, 2019)'
_computing_publication_material  'CIFTab (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.981
_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   -110.00 -16.00   1.00    1.00    --  -40.91 -57.00 -60.00   94
  2  \w    -97.00 -13.00   1.00    1.00    --  -40.91 -57.00  90.00   84
  3  \w   -115.00 -16.00   1.00    1.00    --  -40.91 -38.00-180.00   99
  4  \w     48.00  85.00   1.00    1.00    --   40.91-125.00 -90.00   37
  5  \w      2.00  72.00   1.00    1.00    --   40.91 -99.00  60.00   70
  6  \w     45.00  83.00   1.00    4.00    --  112.00 -45.00 -60.00   38
  7  \w    120.00 178.00   1.00    4.00    --  112.00  77.00  90.00   58
  8  \w     49.00 118.00   1.00    4.00    --  112.00-125.00 -90.00   69
  9  \w     94.00 153.00   1.00    4.00    --  112.00 125.00  30.00   59
 10  \w     35.00 109.00   1.00    4.00    --  112.00 -94.00 -60.00   74
 11  \w     86.00 167.00   1.00    4.00    --  112.00  45.00 150.00   81
 12  \w     36.00 140.00   1.00    4.00    --  112.00 -30.00 -30.00  104
 13  \w    111.00 138.00   1.00    4.00    --  112.00  30.00-120.00   27
 14  \w     64.00  91.00   1.00    4.00    --  112.00-125.00-150.00   27
 15  \w     33.00 101.00   1.00    4.00    --  112.00 -94.00 120.00   68
 16  \w     48.00 125.00   1.00    4.00    --  112.00 -30.00  90.00   77
 17  \w     58.00 112.00   1.00    4.00    --  112.00-125.00  90.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0143
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_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       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4427
_diffrn_reflns_point_group_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.200
_diffrn_reflns_theta_min         4.815
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.623
_exptl_absorpt_correction_T_max  0.494
_exptl_absorpt_correction_T_min  0.190
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            'clear intense green'
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_description       plate
_exptl_crystal_F_000             734
_exptl_crystal_size_max          0.461
_exptl_crystal_size_mid          0.322
_exptl_crystal_size_min          0.151
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 1113 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_coef       0.00061(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2606
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0247
_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^)+(0.0493P)^2^+0.9429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0654
_reflns_Friedel_coverage         0.763
_reflns_Friedel_fraction_full    0.890
_reflns_Friedel_fraction_max     0.836
_reflns_number_gt                2591
_reflns_number_total             2606
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01649g2.cif
_cod_data_source_block           c4
_cod_depositor_comments
'Adding full bibliography for 7704565--7704573.cif.'
_cod_original_sg_symbol_H-M      'I 2'
_cod_database_code               7704568
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.150
_shelx_estimated_absorpt_t_max   0.435
_shelx_res_checksum              87802