(S)-BINOL-derived chiral picolinate ligand as a platform for new polymer frameworks: a pilot study on the effect of the binaphthyl scaffold vs. picolinate
Rodríguez, Humberto A.; Cruz, Daniel A.; Padrón, Juan I.; Lorenzo-Luis, Pablo; New Journal of Chemistry 49 (2025) 12940–12947; doi:10.1039/D5NJ01654A

data_7063862
_publ_section_title
;
 (S)-BINOL-derived chiral picolinate ligand as a platform for new polymer
 frameworks: a pilot study on the effect of the binaphthyl scaffold vs.
 picolinate
;
_journal_issue                   30
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12940
_journal_page_last               12947
_journal_paper_doi               10.1039/D5NJ01654A
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C36 H27 N6 O12 Zn2, C F3 O3 S'
_chemical_formula_sum            'C37 H27 F3 N6 O15 S Zn2'
_chemical_formula_weight         1015.44
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2024-12-12
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-12-12 deposited with the CCDC.	2025-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   13.5985(3)
_cell_length_b                   13.5985(3)
_cell_length_c                   6.08630(10)
_cell_measurement_reflns_used    4929
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.5130
_cell_measurement_theta_min      2.9840
_cell_volume                     974.69(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.136a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.136a 64-bit (release 23-08-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.136a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1268
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f     14.00  86.00   1.00    5.00 -15.00 -15.81  60.00    --    72
  2  \f     86.00 158.00   1.00    5.00 -15.00 -15.81   0.00    --    72
  3  \w     84.00 110.00   1.00   10.00    --   25.49 178.00 150.00   26
  4  \w     65.00 107.00   1.00   10.00    --   25.49 178.00  30.00   42
  5  \w     -9.00  61.00   1.00   10.00    --   25.49 -77.00 150.00   70
  6  \w    -49.00  55.00   1.00   10.00    --  -26.90   0.00  60.00  104
  7  \w    -64.00 -39.00   1.00   10.00    --  -26.90-178.00-180.00   25
  8  \w     55.00  92.00   1.00   10.00    --   25.49  57.00 -90.00   37
  9  \w     22.00  49.00   1.00   10.00    --   25.49  57.00 -90.00   27
 10  \w     82.00 110.00   1.00   10.00    --   25.49 178.00-180.00   28
 11  \w   -118.00 -92.00   1.00   10.00    --  -26.90 178.00-120.00   26
 12  \w    -87.00 -48.00   1.00   10.00    --  -26.90 178.00-120.00   39
 13  \w    -86.00   9.00   1.00   10.00    --  -26.90 -37.00  30.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, EosS2'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0144540000
_diffrn_orient_matrix_UB_12      -0.0578505000
_diffrn_orient_matrix_UB_13      -0.0031074000
_diffrn_orient_matrix_UB_21      -0.0569127000
_diffrn_orient_matrix_UB_22      -0.0159352000
_diffrn_orient_matrix_UB_23      -0.0259622000
_diffrn_orient_matrix_UB_31      0.0134119000
_diffrn_orient_matrix_UB_32      0.0052134000
_diffrn_orient_matrix_UB_33      -0.1135418000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            9243
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.339
_diffrn_reflns_theta_min         1.729
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.380
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.624
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.136a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_description       block
_exptl_crystal_F_000             514
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1526
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0289P)^2^+0.4957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0710
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1416
_reflns_number_total             1526
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj01654a2.cif
_cod_data_source_block           hb_6b
_cod_depositor_comments
'Adding full bibliography for 7063861--7063863.cif.'
_cod_original_cell_volume        974.69(5)
_cod_database_code               7063862
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C16 H16 N2 O6 Zn'
_shelx_estimated_absorpt_t_max   0.898
_shelx_estimated_absorpt_t_min   0.751
_olex2_refinement_description
;
1. Rigid body (RIGU) restrains
 C11
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
2. Others
 Fixed Sof: C11(0.166667) O11(0.5) F11(0.5)
;
_shelx_res_checksum              597
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.192
_oxdiff_exptl_absorpt_empirical_full_min 0.820