Hydrogen bonding regulation-oriented design of pyridine sulfonate as a promising UV birefringent crystal characterized by enhanced structural anisotropy.
Xu, Longyun; Li, Conggang; Li, Shuaifeng; Zhao, Huijian; Kong, Xianghao; Qu, Zaixin; Feng, Wenjie; Xu, Kaidong; Ye, Ning; Hu, Zhanggui; Chemical science 16 (2025) 5186–5193; doi:10.1039/d4sc08583c

data_1573948
_publ_section_title
;
 Hydrogen bonding regulation-oriented design of pyridine sulfonate as a
 promising UV birefringent crystal characterized by enhanced structural
 anisotropy.
;
_journal_issue                   12
_journal_name_full               'Chemical science'
_journal_page_first              5186
_journal_page_last               5193
_journal_paper_doi               10.1039/d4sc08583c
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C10 H16 Ca N2 O10 S2'
_chemical_formula_sum            'C10 H16 Ca N2 O10 S2'
_chemical_formula_weight         428.45
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-08-23
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-12-04 deposited with the CCDC.	2025-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                67.534(14)
_cell_angle_beta                 89.112(15)
_cell_angle_gamma                88.670(15)
_cell_formula_units_Z            2
_cell_length_a                   6.986(3)
_cell_length_b                   11.274(5)
_cell_length_c                   11.590(5)
_cell_measurement_reflns_used    4601
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      24.805
_cell_measurement_theta_min      2.917
_cell_volume                     843.3(6)
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0668
_diffrn_reflns_av_unetI/netI     0.0570
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20058
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         1.90
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.674
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6694
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0929 before and 0.0606 after correction.
The Ratio of minimum to maximum transmission is 0.8978.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             444
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3880
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+0.5762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0895
_reflns_number_gt                2748
_reflns_number_total             3880
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d4sc08583c2.cif
_cod_data_source_block           s1
_cod_depositor_comments          'Adding full bibliography for 1573948.cif.'
_cod_database_code               1573948
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 Ca01-H7A \\sim Ca01-H7B
 with sigma of 0.02
3.a Free rotating group:
 O7(H7A,H7B)
3.b Rotating group:
 O8(H8A), O9(H9A,H9B)
3.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C10(H10), C3(H3), C7(H7), C1(H1), C5(H5), C8(H8), C2(H2)
;
_olex2_submission_special_instructions 'No special instructions were received'