Induction of helical chirality in tetrahedral transition metal complexes with non-bridging monodentate oxazolines.
Bakija, Marija; Perić, Berislav; Rinkovec, Tamara; Sanders, Ernest; Kokan, Zoran; Štefanić, Zoran; Vianello, Robert; Kirin, Srećko I; Dalton transactions (Cambridge, England : 2003) 54 (2025) 17083–17101; doi:10.1039/d5dt02399h

data_7719826
_publ_section_title
;
 Induction of helical chirality in tetrahedral transition metal complexes
 with non-bridging monodentate oxazolines.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17083
_journal_page_last               17101
_journal_paper_doi               10.1039/d5dt02399h
_journal_volume                  54
_journal_year                    2025
_chemical_absolute_configuration syn
_chemical_formula_moiety         '3(C30 H24 Br2 F2 N2 O2 Zn), C2 H3 N'
_chemical_formula_sum            'C92 H75 Br6 F6 N7 O6 Zn3'
_chemical_formula_weight         2164.16
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-09-18 deposited with the CCDC.	2025-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.495(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.3881(3)
_cell_length_b                   7.6278(2)
_cell_length_c                   28.2622(5)
_cell_measurement_reflns_used    20575
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      78.3120
_cell_measurement_theta_min      4.6610
_cell_volume                     4375.04(15)
_computing_cell_refinement       'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            35198
_diffrn_reflns_point_group_measured_fraction_full 0.861
_diffrn_reflns_point_group_measured_fraction_max 0.805
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.667
_diffrn_reflns_theta_min         3.142
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.755
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.101a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            coluorless
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_description       rod
_exptl_crystal_F_000             2156
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.474
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
;
 Flack x determined using 4692 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1082
_refine_ls_number_reflns         15337
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0718P)^2^+4.2278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1307
_reflns_Friedel_coverage         0.547
_reflns_Friedel_fraction_full    0.705
_reflns_Friedel_fraction_max     0.617
_reflns_number_gt                14115
_reflns_number_total             15337
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02399h4.cif
_cod_data_source_block           Zn_1F2_Br2
_cod_depositor_comments
'Adding full bibliography for 7719815--7719833.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7719826
_shelx_shelxl_version_number     2019/3
_shelx_res_checksum              50198
_shelx_hkl_checksum              56562