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_7704571
_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 Cl4 Cu N2 O2'
_chemical_formula_sum            'C30 H24 Cl4 Cu N2 O2'
_chemical_formula_weight         649.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 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                 97.2834(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.57142(6)
_cell_length_b                   14.70541(11)
_cell_length_c                   11.09232(8)
_cell_measurement_reflns_used    8501
_cell_measurement_temperature    140.01(10)
_cell_measurement_theta_max      75.8270
_cell_measurement_theta_min      3.9980
_cell_volume                     1386.864(18)
_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      140.01(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 0.976
_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    -64.00  32.00   1.00    1.00    --  -40.91  57.00   0.00   96
  2  \w    -32.00  -5.00   1.00    1.00    --  -40.91 125.00  30.00   27
  3  \w      5.00  54.00   1.00    1.00    --   40.91 -99.00  90.00   49
  4  \w     39.00 134.00   1.00    4.00    --  111.85 -45.00 -60.00   95
  5  \w     85.00 178.00   1.00    4.00    --  111.85  30.00  30.00   93
  6  \w    101.00 139.00   1.00    4.00    --  111.85 125.00 -60.00   38
  7  \w     85.00 178.00   1.00    4.00    --  111.85  30.00 120.00   93
  8  \w     66.00 109.00   1.00    4.00    --  111.85 -94.00 150.00   43
  9  \w     53.00 108.00   1.00    4.00    --  111.85 -94.00  60.00   55
 10  \w     70.00 141.00   1.00    4.00    --  111.85 -61.00  30.00   71
 11  \w     63.00  93.00   1.00    4.00    --  111.85 -94.00-120.00   30
 12  \w     36.00 109.00   1.00    4.00    --  111.85 -30.00-150.00   73
 13  \w     55.00  96.00   1.00    1.00    --   40.91-125.00-150.00   41
 14  \w     47.00 110.00   1.00    4.00    --  111.85-100.00 -41.00   63
 15  \w     43.00 118.00   1.00    4.00    --  111.85 -45.00 150.00   75
 16  \w    -85.00 -59.00   1.00    1.00    --  -40.91 125.00  30.00   26
 17  \w   -115.00 -16.00   1.00    1.00    --  -40.91 -38.00 120.00   99
 18  \w   -111.00 -26.00   1.00    1.00    --  -40.91 -38.00-150.00   85
;
_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     0.0174
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9280
_diffrn_reflns_point_group_measured_fraction_full 0.896
_diffrn_reflns_point_group_measured_fraction_max 0.859
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.011
_diffrn_reflns_theta_min         4.018
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.917
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark black'
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_description       prism
_exptl_crystal_F_000             662
_exptl_crystal_size_max          0.543
_exptl_crystal_size_mid          0.247
_exptl_crystal_size_min          0.175
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.010(11)
_refine_ls_extinction_coef       0.0033(3)
_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   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         4988
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0251
_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^)+(0.0509P)^2^+0.2627P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0655
_reflns_Friedel_coverage         0.692
_reflns_Friedel_fraction_full    0.782
_reflns_Friedel_fraction_max     0.732
_reflns_number_gt                4980
_reflns_number_total             4988
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01649g2.cif
_cod_data_source_block           gb7
_cod_depositor_comments
'Adding full bibliography for 7704565--7704573.cif.'
_cod_original_cell_volume        1386.863(18)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7704571
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.175
_shelx_estimated_absorpt_t_max   0.480
_shelx_res_checksum              90337