Synergistic engineering of ultraviolet metal-free crystals with exceptional birefringence <i>via</i> pyridine-derived dimers.
Lu, Jiachen; Ok, Kang Min; Chemical science 16 (2025) 4703–4709; doi:10.1039/d5sc00112a

data_1573850
_publ_section_title
;
 Synergistic engineering of ultraviolet metal-free crystals with
 exceptional birefringence <i>via</i> pyridine-derived dimers.
;
_journal_issue                   11
_journal_name_full               'Chemical science'
_journal_page_first              4703
_journal_page_last               4709
_journal_paper_doi               10.1039/d5sc00112a
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C5 H4 N O3 S, C5 H5 N O, C5 H6 N O'
_chemical_formula_sum            'C15 H15 N3 O5 S'
_chemical_formula_weight         349.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-25
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-10-25 deposited with the CCDC.	2025-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.8810(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5972(5)
_cell_length_b                   7.0455(2)
_cell_length_c                   12.8268(3)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    303.00
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      3.11
_cell_volume                     1590.09(7)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      303.00
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            29324
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.315
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.235
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6527
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0853 before and 0.0774 after correction.
The Ratio of minimum to maximum transmission is 0.8753.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       plate
_exptl_crystal_F_000             728
_refine_diff_density_max         0.167
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         2795
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0343P)^2^+0.9257P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0983
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2385
_reflns_number_total             2795
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc00112a2.cif
_cod_data_source_block           x_CCDC1
_cod_depositor_comments
'Adding full bibliography for 1573849--1573850.cif.'
_cod_database_code               1573850
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups
2.a Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_shelx_res_checksum              37114
_shelx_hkl_checksum              94932
_olex2_submission_special_instructions 'No special instructions were received'